TY - CONF
A1 - Cakir, Cafer Tufan
T1 - High Speed for High Entropy Materials
N2 - Time is the most valuable parameter in synchrotron experiments. This is costly and some of the experiments suffer from low efficiency due to low counting statistics. With today's high processing power long experiments are run in a shorter time and increase efficiency. With optimization algorithms time in "counting-hungry" experiments reduced by factor of 10. Our project is to develop a new method to analyze the chemical properties of complex materials non-destructively and efficiently, such as high entropy materials subjected to corrosion processes. A better understanding of the corrosion process will help to develop corrosion-resistant materials and reduce the cost of corrosion damage, which averages around 2.5 trillion USD annually.
T2 - Berlin Science Week
CY - Berlin, Germany
DA - 01.11.2022
KW - GEXRF
KW - High entropy alloys
KW - XANES
KW - High entropy materials
KW - Grazing exit
KW - XAS
KW - Optimization
PY - 2022
AN - OPUS4-56269
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - CONF
A1 - Cakir, Cafer Tufan
T1 - Optimization of Depth Resolved X-Ray Absorption Spectroscopy in Grazing Emission Mode for Characterizing Compositionally Complex Alloys
N2 - The components that are used in structural and in high temperature applications generally face significant challenges with respect to oxidation behaviours and metalworking processes. In most of the cases, harsh environmental conditions lead materials to degrade due to corrosion. To thoroughly investigate the corrosion processes and to determine oxidation states of metal components within the reaction products, we need special analytical tools. Grazing exit X-ray fluorescence (GEXRF) offers a non-destructive way to collect this information in sub-micrometre depth range.
In order to obtain structural information, such as regarding oxidation states or atomic/molecular geometric arrangement, the GEXRF approach can also be combined with the X-ray absorption spectroscopy (XAS) method. The position and energy sensitive detector, with 264x264 pixel detector area, provides information regarding the signal emitted from the sample as a function of the emission angle and thus allows depth-sensitive analysis. Furthermore, the data collected from samples of an incidence energy which can be controlled with a resolution of 0.5 eV provides XANES data to determine oxidation states.
We address the feasibility of our setup and provide a new optimization procedure (Bayesian Optimization and Gaussian Regression) to decrease measuring time. The results settle on a conceptual study on a reference sample (Cr-Oxide layer (300nm) on Cr layer (500nm) on Si wafer).
T2 - XAFS 2022, The 19th International XAFS Conference
CY - Sydney, Australia
DA - 10.07.2022
KW - GEXRF
KW - High entropy alloys
KW - XANES
KW - Grazing exit
KW - High entropy materials
KW - Optimization
KW - XAS
PY - 2022
AN - OPUS4-56270
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - CONF
A1 - Radtke, Martin
T1 - Energy Resolved Imaging with Coded Apertures
N2 - Our aim is to develop a simple and inexpensive method for full field X-ray fluorescence imaging.We combine an energydispersive array detector with a coded aperture to obtain high resolut ion images. To obtain the information from the recorded image a reconstruction step is necessary. The reconstruction methods we have developed, were tested on simulated data and then applied to experimental data. The first tests were carried out at the BAMline @BESSY II. This method enables the simultaneous detection of multiple elements,which is important e.g. in the field of catalysis.
T2 - SRI 2021
CY - Online meeting
DA - 28.3.2022
KW - Synchrotron
KW - BAMline
KW - Machine Learning
KW - Coded Aperture
PY - 2022
AN - OPUS4-56298
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - CONF
A1 - Heilmann, Maria
T1 - Size-Tunable Ni-Cu Core-Shell Nanoparticles: Structure, Composition, and Catalytic Activity
N2 - Nanoparticles (NPs) have become important materials for a variety of chemical technologies, including catalysis. One of the main challenges is the reduction of green house gases, such as CO2. One opportunity besides the capturing is the conversion to synthesis gas via the reverse water-gas shift reaction.
A facile and efficient method is described for the solvothermal synthesis of size-tunable, stable, and uniform NiCu core-shell NPs. The diameter of the NPs can be tuned in a range from 6 nm to 30 nm and the Ni:Cu ratio from 30:1 to 1:1. The NPs are structurally characterized with combination of transmission electron microscopy, anomalous small-angle X-ray scattering, X-ray photoelectron spectroscopy, and X-ray absorption fine structure. Using these analytical methods, a core-shell-shell structure their chemical composition is elucidated. A depletion from the core to the shell is observed, with the core consisting of NiCu alloy, surrounded by an inner Ni-rich shell and an outer NiO shell. The SiO2-supported NiCu core-shell NPs show pronounced selectivity of >99% for CO in the catalytic reduction of CO2 to CO using hydrogen as reactant (reverse water–gas shift reaction).
T2 - Nanoalloys: recent developments and future perspectives Faraday Discussion
CY - London, UK
DA - 21.09.2022
KW - Nanoparticles
KW - Core-shell
KW - Catalysis
PY - 2022
AN - OPUS4-56831
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - CONF
A1 - Linberg, Kevin
T1 - Polymorphism in molecular cocrystals controlled by variable temperature ball milling
N2 - Mechanochemistry offers a unique opportunity to modify or synthesize new crystal forms. Although the method is very promising, little is known about the mechanochemical means to control the synthesis of a solid form. Using an polymorphic organic cocrystal system, we show here that mechanochemistry can be used to obtain a polymorph transformation under the apparently conventional (thermal) transition point.
T2 - Bessy User Meeting 2022
CY - Online meeting
DA - 08.12.2022
KW - Mechanochemistry
KW - Polymorphism
KW - TRIS
PY - 2022
AN - OPUS4-56473
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - CONF
A1 - Dalgic, Mete-Sungur
T1 - Einfluss der Konformation auf das Ionisationsverhalten in MALDI-TOF MS
N2 - MALDI-TOF Massenspektrometrie ist eine wichtige Methode zur Bestimmung von Molekulargewichten von Polymeren. Jedoch wird die quantitative Analyse von Polymeren durch verschiedene Faktoren erschwert. In dieser Präsentation wird unter anderem der Einfluss der molaren Massen auf die Massenspektren näher betrachtet. Dabei werden Konturplots von ternären PMMA- und PS-Mischungen gezeigt.
T2 - 27. Kolloquium - Massenspetrometrische von Polymeren
CY - Berlin, Germany
DA - 09.05.2023
KW - MALDI-TOF MS
KW - Ternäre Polymermischungen
KW - PMMA und PS
PY - 2023
AN - OPUS4-62214
LA - deu
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - GEN
A1 - Pauw, Brian Richard
A1 - Röder, Bettina
A1 - Smales, Glen Jacob
T1 - High temperature in-vacuum flow-through sample holder (sandwich design version 1.1)
N2 - Technical drawings and documents for building a compact, heated, vacuum compatible flow-through sample holder. This holder is in use at the BAM MOUSE instrument as well as at the I22 beamline at the Diamond Light Source (see references for instrument details).
This holder has several features:
- The holder can be used in vacuum environments as well as in atmosphere
- It has two G 1/4" UNF fittings to attach HPLC tubing for (optionally) flowing a medium through the sample cell
- There are two additional (unflowed) sample positions for backgrounds and calibrants, held at the same temperature
- The low-mass design coupled with a 250W heating element can achieve heating rates of 1 degree C per second, when coupled (for example) with an Omron E5CC PID controller.
- The sample holder insert can be made from various materials depending on the application. Sealing the sample from the vacuum can be achieved using kapton, teflon or Magic tape, depending on the temperature requirements. The inlet and outlet holes will need to be punctured with a needle to enable flow.
- Large exit cones ensure a clear exit angle of at least 45 degrees two theta.
- It has been tested with temperatures up to 400 degrees C.
- Compression area has been raised and polished to ensure a good vacuum seal.
KW - SAXS
KW - X-ray scattering
KW - Sample cell
KW - Sample holder
KW - Heated
KW - Flow-through
KW - Vacuum compatible
KW - XRD
KW - WAXS
PY - 2023
DO - https://doi.org/10.5281/zenodo.7501030
PB - Zenodo
CY - Geneva
AN - OPUS4-56777
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Becker, Roland
A1 - Scholz, Philipp
A1 - Jung, Christian
A1 - Weidner, Steffen
T1 - Thermo-Desorption Gas Chromatography-Mass Spectrometry for investigating the thermal degradation of polyurethanes
N2 - Thermo-Desorption Gas Chromatography-Mass Spectrometry (TD-GC-MS) was used to investigate the thermal degradation of two different polyurethanes (PU). PU samples were heated at different heating rates and the desorbed products were collected in a cold injection system and thereafter submitted to GC-MS. Prospects and limitations of the detection and quantification of semi-volatile degradation products were investigated. A temperature dependent PU depolymerization was
found at temperatures above 200 °C proved by an increasing release of 1,4-butanediol and methylene diphenyl diisocyanate (MDI) representing the main building blocks of both polymers. Their release was monitored quantitatively based on external calibration with authentic compounds. Size Exclusion Chromatography (SEC) of the residues obtained after thermodesorption confirmed the initial competitive degradation mechanism indicating an equilibrium of crosslinking and depolymerization as previously suggested. Matrix-Assisted Laser Desorption Ionization (MALDI) mass spectrometry of SEC fractions of thermally degraded PUs provided additional hints on degradation mechanism.
KW - Thermo-desorption
KW - Mass spectrometry
KW - Polyurethanes
KW - Thermal degradation
PY - 2023
DO - https://doi.org/10.1039/D3AY00173C
SN - 1759-9660
SP - 1
EP - 6
PB - Royal Society for Chemistry
AN - OPUS4-57307
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - CONF
A1 - Pollack, M.
T1 - Functionalized poly(ethylene glycol)s (PEGs) as a reference material for detection of polymeric end groups via SEC hyphenated with FTIR and 1H-NMR (80 MHz)
N2 - Benchtop 1H-NMR and FTIR have both been successfully developed for size-exclusion chromatography (SEC) applications. The latest implementations of these methods by Wilhelm and collaborators[1-3] have taken advantage of commerically available low-cost equipment, and a provide a means to obtain slice-by-slice spectra for the monitoring of functional groups in polymer separations. Demonstrated applications include the detection of highly diluted chains in a polymer blend (e.g., PS/PMMA), copolymer content determination (e.g., styrene-methyl methacrylate), and butadiene isomer detection. To synthesize and characterize an end-labelled low molecular wt. poly(ethylene glycol) as a model polymer to aid in the development and validation of spectroscopic detection (FTIR and 1H-NMR) for SEC applications. A particular focus is to improve quantitation and/or detection of highly diluted funtional groups (e.g., polymer chain ends or sparsely functionalized chains) In the first approach, an isocyanate with IR- and NMR-active functional groups was reacted with PEG (4000 and 10000 g/mol) to form end-functionalized chains by means of an addition reaction. The functionalization of the 10000 g/mol PEG was found to be non-homogeneous (not discussed further). The 4000 g/mol PEG was successfully functionalized to 100%, found to be homogeneous across the molecular weight distribution and could therefore serve as a model polymer for analysis by the coupled methods.
T2 - 10th International Symposium on the Separation and Charcterization of Natural and Synthetic Macromolecules
CY - Amsterdam, Netherlands
DA - 01.02.2023
KW - PEG
KW - Reference materials
KW - NMR
KW - MALDI-TOF MS
PY - 2023
AN - OPUS4-57071
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Nguyen, H. G.
A1 - Toman, B.
A1 - van Zee, R.
A1 - Prinz, Carsten
A1 - Thommes, M.
A1 - Ahmad, R.
A1 - Kiska, D.
A1 - Salinger, J.
A1 - Walton, I.
A1 - Walton, K.
A1 - Broom, D.
A1 - Benham, M.
A1 - Ansari, H.
A1 - Pini, R.
A1 - Petit, C.
A1 - Adolphs, J.
A1 - Schreiber, A.
A1 - Shigeoka, T.
A1 - Konishi, Y.
A1 - Nakai, K.
A1 - Henninger, M.
A1 - Petrzik, T.
A1 - Kececi, C.
A1 - Martis, V.
A1 - Paschke, T.
A1 - Mangano, E.
A1 - Brandani, S.
T1 - Reference isotherms for water vapor sorption on nanoporous carbon: results of an interlaboratory study
N2 - This paper reports the results of an international interlaboratory study sponsored by the Versailles Project on Advanced Materials and Standards (VAMAS) and led by the National Institute of Standards and Technology (NIST) on the measurement of water vapor sorption isotherms at 25 °C on a pelletized nanoporous carbon (BAM-P109, a certified reference material). Thirteen laboratories participated in the study and contributed nine pure water vapor isotherms and four relative humidity isotherms, using nitrogen as the carrier gas. From these data, reference isotherms, along with the 95% uncertainty interval (Uk=2), were determined and are reported in a tabular format.
KW - BAM-P109
KW - Interlaboratory study
KW - Nanoporous carbon
KW - Reference isotherm
KW - VAMAS
PY - 2023
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-576560
DO - https://doi.org/10.1007/s10450-023-00383-1
SN - 0929-5607
SP - 1
EP - 12
PB - Springer
CY - Heidelberg
AN - OPUS4-57656
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - CONF
A1 - Kossatz, Philipp
T1 - Upconversion Nanoparticles for Luminescent Barcodes and as Reporters for Optical Sensors
N2 - Counterfeiting of goods has serious economic implications worldwide and can be a threat to human health and safety. Upconversion nanoparticles (UCNPs)are ideal candidates for optical encoding of various materials. Particles with tailor-made emission patterns can be used as anti-counterfeiting markers and luminophores in security inks and to track material flows. Microenvironment-specific changes in the emission properties of the UCNP tags can be used to study, signal, and sense changes of physico-chemical parameters in different environments, e.g., building
materials.
T2 - ANAKON 2023
CY - Vienna, Austria
DA - 11.04.2023
KW - Nanomaterials
KW - Anti-Counterfeiting
KW - Fluorescence Spectroscopy
PY - 2023
AN - OPUS4-59035
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - CONF
A1 - Kossatz, Philipp
T1 - Lanthanide Nanocrystals as Authentication and Security Tags and Reporters for Optical Sensors
N2 - Counterfeiting of goods has serious economic implications worldwide and can present a considerable threat to human health and national security, rendering product authentication more and more important. This led to an increasing interest in simple tags for anticounterfeiting and authentication applications for the integration into different materials and matrices that are robust enough to survive the respective production processes and can be read out in-situ with simple instrumentation.
Here we present a platform of chemically inert, multi-color luminescent lanthanide nanocrystals (LnNC) consisting of a NaYF4 matrix doped with Yb, Er, Tm, or Ho as promising candidates for such applications.
LnNC with characteristic multi-color emission patterns, composed of narrow bands of varying intensity in the ultraviolet, visible, near-infrared, and short-wave were synthesized via a thermal decomposition approach under inert conditions[1]. The tailor-made design of different emission pattern was achieved by tuning particle size, material composition, and particle surface chemistry in upscaleable syntheses.[2] Particle size and morphology were determined by dynamic light scattering and transmission electron microscopy and the optical properties were characterized by absorption and fluorescence spectroscopy as well as fluorescence lifetime measurements.
The particles were then incorporated into security inks and consumer products. In addition, microenvironment-specific changes in the emission properties of the LnNC tag were utilized to study and sense changes of physico-chemical parameters in different matrices.
T2 - JCF Frühjahrssymposium 2023
CY - Gießen, Germany
DA - 21.03.2023
KW - Lanthanide Nanocrystals
KW - Anti-Counterfeiting
KW - Fluorescence Spectroscopy
PY - 2023
AN - OPUS4-59037
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Chabbah, T.
A1 - Chatti, S.
A1 - Jaffrezic-Renault, N.
A1 - Weidner, Steffen
A1 - Marestin, C.
A1 - Mercier, R.
T1 - Impedimetric sensors based on diethylphosphonate-containingpoly(arylene ether nitrile)s films for the detection of lead ions
N2 - This article describes the elaboration and characterization of diethylphosphonate-containing polymers coated electrodes as sensors for the detection of heavy metalstraces, by electrochemical impedance spectroscopy. Diethylphosphonate groupswere chosen as heavy metals binding sites. Two different series of polymers bearingthese anchoring groups were synthesized. Whereas the diethylphosphonate groupsare directly incorporated in the aromatic macromolecular chain in some polymers, analiphatic spacer is removing the chelating site from the polymer backbone in others.The influence of the macromolecular structure on the sensing response was studied,especially for the detection of Pb2+,Ni2+,Cd2+and Hg2+. Polymer P6, including thehigher amount of diethylphosphonate groups removed from the polymer chain by ashort alkyl spacer gave the higher sensitivity of detection of lead ions, with a detec-tion limit of 50 pM
KW - Heavy metals
KW - Phosphonate esters
KW - Lead ions
KW - MALDI TOF MS
PY - 2023
DO - https://doi.org/10.1002/pat.6065
SN - 1042-7147
SP - 1
EP - 11
PB - John Wiley & Sons, Ltd
AN - OPUS4-57356
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Lisec, Jan
A1 - Recknagel, Sebastian
A1 - Prinz, Carsten
A1 - Vogel, Kristin
A1 - Koch, Matthias
A1 - Becker, Roland
T1 - eCerto—versatile software for interlaboratory data evaluation and documentation during reference material production
N2 - The statistical tool eCerto was developed for the evaluation of measurement data to assign property values and associated uncertainties of reference materials. The analysis is based on collaborative studies of expert laboratories and was implemented using the R software environment. Emphasis was put on comparability of eCerto with SoftCRM, a statistical tool based on the certification strategy of the former Community Bureau of Reference. Additionally, special attention was directed towards easy usability from data collection through processing, archiving, and reporting. While the effects of outlier removal can be flexibly explored, eCerto always retains the original data set and any manipulation such as outlier removal is (graphically and tabularly) documented adequately in the report. As a major reference materials producer, the Bundesanstalt für Materialforschung und -prüfung (BAM) developed and will maintain a tool to meet the needs of modern data processing, documentation requirements, and emerging fields of RM activity. The main features of eCerto are discussed using previously certified reference materials.
KW - Reference material
KW - Statistics
KW - Software
KW - Collaborative trial
PY - 2023
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-591851
DO - https://doi.org/10.1007/s00216-023-05099-3
SP - 1
EP - 9
PB - Springer Science and Business Media LLC
AN - OPUS4-59185
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - CONF
A1 - Kossatz, Philipp
T1 - Upconversion Nanoparticles as Luminescent Probes for Cement
N2 - Safety is a key parameter for the design and construction of buildings. The most widely used construction material to date is concrete that consists of about 15-20 wt.-% cement, which is responsible for the main concrete properties, i.e., strength and durability. Despite many standards regulating the quality of cement, at present, there exists no viable method to track the cement life cycle “from cradle to grave”. This led to an increasing interest in simple and robust methods for studying the processes and changes occurring during the life cycle of cement. In this context, we explored the applicability of fluorescence measurements which can be performed with relatively inexpensive and miniaturized instrumentation yet require robust optical probes which survive the harsh cement environment. Therefore, we developed a platform of lanthanide-based upconversion nanoparticles (UCNPs), consisting of a NaYF4 matrix doped with Yb3+ and Er3+ with sizes between 20 nm and 55 nm, which show characteristic multi-color emission patterns, composed of narrow bands of varying intensity in the ultraviolet, visible, near-infrared, and short-wave spectral region and examined their potential for cement probing and the non-invasive monitoring of the hydration processes occurring during cement formation.
UCNPs of different size and chemical composition were synthesized via a thermal decomposition approach under inert conditions. The tailor-made design of different emission patterns was achieved by tuning particle size and morphology, material composition, and particle surface chemistry in upscaleable syntheses. For cement probing, different types of UCNPs were added to cement and the evolution of the UCNP emission pattern was used to probe in-situ changes of physico-chemical parameters in the cementitious environment during hydration, utilizing a simple and portable custom-designed optical setup. The observed changes in the UCNP emission patterns are characteristic for a given particle size, surface chemistry, and cement composition. In addition to fluorescence measurements, conventional isothermal heat flow calorimetry was used to study the influence of UCNP addition on cement hydration kinetics. Subsequently, both sets of measurements were correlated. Our results underline the potential of our optical approach ad UCNPs for the non-invasive probing of cementitious systems and cement hydration. This can be also exploited for cutting-edge applications of construction materials such as 3D concrete printing.
T2 - Summer School Exciting Nanostructures
CY - Bad Honnef, Germany
DA - 31.07.2023
KW - Cement Hydration
KW - Upconversion
KW - Fluorescence Spectroscopy
PY - 2023
AN - OPUS4-58203
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - GEN
A1 - Radnik, Jörg
A1 - Chemello, Giovanni
A1 - Knigge, Xenia
A1 - Al-Sabbgh, Dominik
A1 - Hodoroaba, Vasile-Dan
T1 - XPS, HAXPES, XRD and SEM datasets of functionalized graphene nanoplateletes
N2 - The datasets from (Hard Energy) X-ray photoelectron spectroscopy, X-ray diffraction and Scanning Electron Microsopy are related to the publication
G. Chemello, X. Knigge, D. Ciornii, B.P. Reed, A.J. Pollard, C.A. Clifford, T. Howe, N. Vyas, V.-D. Hodoroaba, J. Radnik
"Influence of the morphology on the functionalization of graphene nanoplatelets analyzed by comparative photoelectron spectroscopy with soft and hard X-rays"
Advanced Materials Interfaces (2023), DOI: 10.1002/admi.202300116.
KW - Graphene related 2D materials
KW - X-ray photoelectron spectroscopy
KW - Hard-energy X-ray photoelectron spectroscopy
KW - Scanning electron microscopy
KW - Powder X-ray diffraction
PY - 2023
DO - https://doi.org/10.5281/zenodo.7956497
PB - Zenodo
CY - Geneva
AN - OPUS4-57898
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Guerra, M.F.
A1 - Neri, E.
A1 - Radtke, Martin
T1 - Gold leaf tesserae: tracing the origins of gold using synchrotron-based techniques
N2 - To gain insight into the possible origin of the gold used in the production of tesserae containing gold leaf less than 0.5 μm thick placed between two layers of glass, we propose a non-destructive synchrotron radiation (SR) XRF protocol based on sequential analysis under optimised analytical conditions. Using this protocol, trace element analysis is achieved with detection limits of 1–6 mg/kg. As Pt and Au have adjacent fluorescence energies, we tested the most challenging situation, when Pt is present in very low concentrations in gold. Data obtained by double-dispersive XRF (D2XRF) and μXRF for fourth–ninth-century mosaics decorating nine Eastern and Western religious buildings show that the Eastern and Western tesserae are made from different alloys.
However, these alloys are identical to those used to make gold leaf for gilding, because plastic deformation requires the use of gold alloys with high ductility and malleability. Although trace element composition of gold used in the concerned period is only available for coins, by comparing the amounts of Pt contained in the tesserae and in the coins we show that Roman tesserae are made from Roman gold, as described in the documentary sources. We observe for the Byzantine period the use of a Byzantine gold and of gold supposedly from different stages of recycling, and we suggest the use of Umayyad and Abbasid gold for the production of Islamic tesserae.
KW - Gold
KW - XRF
KW - Synchrotron
KW - BAMline
KW - D2XRF
KW - Tesserae
PY - 2023
DO - https://doi.org/10.1140/epjp/s13360-022-03638-y
SN - 2190-5444
VL - 138
IS - 2
SP - 1
EP - 15
AN - OPUS4-57208
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - CONF
A1 - Radtke, Martin
T1 - Enhancing efficiency at bamline: employing data science and machine learning for x-ray research
N2 - This talk discusses how data science and machine learning techniques are being applied at the BAM Federal Institute for Materials Research and Testing to enhance efficiency and automation at the BAMLine synchrotron facility. The methods presented include Gaussian processes and Bayesian optimization for beamline adjustment and optimization of X-ray measurements. These statistical techniques allow automated alignment of beamline components and active learning scanning to reduce measurement time.
Additional machine learning methods covered are neural networks for quantification of X-ray fluorescence (XRF) data and decoding coded apertures.
T2 - 17th International Work-Conference on Artificial Neural Networks (IWANN2023)
CY - Ponta Delgada, Portugal
DA - 19.06.2023
KW - Bayesian Optimization
KW - Gaussian Process
KW - BAMline
PY - 2023
AN - OPUS4-58605
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Pauw, Brian Richard
A1 - Smales, Glen Jacob
A1 - Anker, A. S.
A1 - Annadurai, V.
A1 - Balazs, D. M.
A1 - Bienert, Ralf
A1 - Bouwman, W. G.
A1 - Breßler, Ingo
A1 - Breternitz, J.
A1 - Brok, E. S.
A1 - Bryant, G.
A1 - Clulow, A. J.
A1 - Crater, E. R.
A1 - De Geuser, F.
A1 - Del Giudice, A.
A1 - Deumer, J.
A1 - Disch, S.
A1 - Dutt, S.
A1 - Frank, K.
A1 - Fratini, E.
A1 - Garcia, P. R. A. F.
A1 - Gilbert, E. P.
A1 - Hahn, Marc Benjamin
A1 - Hallett, J.
A1 - Hohenschutz, M.
A1 - Hollamby, M.
A1 - Huband, S.
A1 - Ilavsky, J.
A1 - Jochum, J. K.
A1 - Juelsholt, M.
A1 - Mansel, B. W.
A1 - Penttilä, P.
A1 - Pittkowski, R. K.
A1 - Portale, G.
A1 - Pozzo, L. D.
A1 - Rochels, L.
A1 - Rosalie, Julian
A1 - Saloga, Patrick E. J.
A1 - Seibt, S.
A1 - Smith, A. J.
A1 - Smith, G. N.
A1 - Spiering, G. A.
A1 - Stawski, Tomasz M.
A1 - Taché, O.
A1 - Thünemann, Andreas
A1 - Toth, K.
A1 - Whitten, A. E.
A1 - Wuttke, J.
T1 - The human factor - Results of a small-angle scattering data analysis round robin
N2 - A round-robin study has been carried out to estimate the impact of the human element in small-angle scattering data analysis. Four corrected datasets were provided to participants ready for analysis. All datasets were measured on samples containing spherical scatterers, with two datasets in dilute dispersions and two from powders. Most of the 46 participants correctly identified the number of populations in the dilute dispersions, with half of the population mean entries within 1.5% and half of the population width entries within 40%. Due to the added complexity of the structure factor, far fewer people submitted answers on the powder datasets. For those that did, half of the entries for the means and widths were within 44 and 86%, respectively. This round-robin experiment highlights several causes for the discrepancies, for which solutions are proposed.
KW - Round Robin
KW - Data analysis
KW - Small-angle scattering
KW - Nanomaterials
KW - Interlaboratory comparability
KW - Nanostructure quantification
KW - Methodology
KW - MOUSE
PY - 2023
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-587091
DO - https://doi.org/10.1107/S1600576723008324
SN - 1600-5767
VL - 56
IS - 6
SP - 1618
EP - 1629
PB - Wiley-Blackwell
CY - Oxford
AN - OPUS4-58709
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - INPR
A1 - Pauw, Brian Richard
A1 - Smales, Glen Jacob
A1 - Anker, A. S.
A1 - Balazs, D. M.
A1 - Beyer, F. L.
A1 - Bienert, Ralf
A1 - Bouwman, W. G.
A1 - Breßler, Ingo
A1 - Breternitz, J.
A1 - Brok, E. S.
A1 - Bryant, G.
A1 - Clulow, A. J.
A1 - Crater, E. R.
A1 - De Geuser, F.
A1 - Giudice, A. D.
A1 - Deumer, J.
A1 - Disch, S.
A1 - Dutt, S.
A1 - Frank, K.
A1 - Fratini, E.
A1 - Gilbert, E. P.
A1 - Hahn, Marc Benjamin
A1 - Hallett, J.
A1 - Hohenschutz, Max
A1 - Hollamby, M. J.
A1 - Huband, S.
A1 - Ilavsky, J.
A1 - Jochum, J. K.
A1 - Juelsholt, M.
A1 - Mansel, B. W.
A1 - Penttilä, P.
A1 - Pittkowski, R. K.
A1 - Portale, G.
A1 - Pozzo, L. D.
A1 - Ricardo de Abreu Furtado Garcia, P.
A1 - Rochels, L.
A1 - Rosalie, Julian
A1 - Saloga, P. E. J.
A1 - Seibt, S.
A1 - Smith, A. J.
A1 - Smith, G. N.
A1 - Annadurai, V.
A1 - Spiering, G. A.
A1 - Stawski, Tomasz
A1 - Taché, O.
A1 - Thünemann, Andreas
A1 - Toth, K.
A1 - Whitten, A. E.
A1 - Wuttke, J.
T1 - The human factor - Results of a small-angle scattering data analysis round robin
N2 - A Round Robin study has been carried out to estimate the impact of the human element in small-angle scattering data analysis. Four corrected datasets were provided to participants ready for analysis. All datasets were measured on samples containing spherical scatterers, with two datasets in dilute dispersions, and two from powders.
Most of the 46 participants correctly identified the number of populations in the dilute dispersions, with half of the population mean entries within 1.5 % and half of the population width entries within 40 %, respectively. Due to the added complexity of the structure factor, much fewer people submitted answers on the powder datasets.
For those that did, half of the entries for the means and widths were within 44 % and 86 % respectively. This Round Robin experiment highlights several causes for the discrepancies, for which solutions are proposed.
KW - Round robin
KW - Sall-angle scattering
KW - Nanostructure quantification
KW - Nanostructure
KW - SAXS
KW - MOUSE
KW - X-ray scattering
KW - Size distribution
KW - Nanoparticles
PY - 2023
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-571342
DO - https://doi.org/10.48550/arXiv.2303.03772
SP - 1
EP - 23
PB - Cornell University
CY - Ithaca, NY
AN - OPUS4-57134
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Förste, F.
A1 - Bauer, L.
A1 - Streeck, C.
A1 - Radtke, Martin
A1 - Reinholz, Uwe
A1 - Kadow, D.
A1 - Keil, C.
A1 - Mantouvalou, I.
T1 - Quantitative Analysis and 2D/3D Elemental Imaging of Cocoa Beans Using X‑ray Fluorescence Techniques
N2 - As an important raw material for the confectionery industry, the cocoa bean (Theobroma cacao L.) has to meet certain legal requirements in terms of food safety and maximum contaminant levels in order to enter the cocoa market. Understanding the enrichment and distribution of essential minerals but also toxic metals is of utmost importance for improving the nutritional quality of this economically important raw food material. We present three X-ray fluorescence (XRF) techniques for elemental bio-imaging of intact cocoa beans and one additional XRF technique for quantitative analysis of cocoa pellets. The interrelation of all the methods presented gives a detailed picture of the content and 3D-resolved distribution of elements in complete cocoa beans for the first time.
KW - BAMline
KW - Synchrotron
KW - XRF
KW - CXC
KW - Cocoa
PY - 2023
DO - https://doi.org/10.1021/acs.analchem.2c05370
VL - 95
SP - 5627
EP - 5635
PB - ACS Publications
AN - OPUS4-57832
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - CHAP
A1 - Radtke, Martin
A1 - Reinholz, Uwe
A1 - Guerra, M.F.
A1 - Martinón-Torres, M.
A1 - Lemasson, Q.
A1 - Moignard, B.
A1 - Pacheco, C.
A1 - Pichon, L.
A1 - Macdonald, L.
A1 - Hess, M.
A1 - Tissot, I.
ED - Guerra, M. F.
ED - Martinón-Torres, M.
ED - Quirke, S.
T1 - Analytical approaches to Egyptian goldwork
N2 - The structure and composition of ancient gold objects retain information about their long history of manufacture, from the exploitation of the ore to the finishing touches, as well as evidence of their use, deposition, and degradation. By developing an efficient analytical strategy, it is possible to retrieve that information. This chapter sets the necessary foundation 131to explore fully the analytical results presented in the following chapters of this volume. The techniques employed in the analyses of the Egyptian jewellery are described and the analytical parameters provided. For more established techniques, only brief introductions are presented, while more recent developments are presented in greater detail.
KW - Gold
KW - Synchrotron
KW - D2XRF
KW - Egypt
PY - 2023
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-586039
DO - https://doi.org/10.17863/CAM.99681
SP - 131
EP - 191
AN - OPUS4-58603
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Tannenberg, Robert
A1 - Paul, Martin
A1 - Röder, Bettina
A1 - Gande, S. L.
A1 - Sreeramulu, S.
A1 - Saxena, K.
A1 - Richter, C.
A1 - Schwalbe, H.
A1 - Swart, C.
A1 - Weller, Michael G.
T1 - Chemiluminescence biosensor for the determination of cardiac troponin I (cTnI)
N2 - Cardiac troponin I (cTnI) is a crucial biomarker for diagnosing cardiac vascular diseases, including acute myocardial infarction (AMI). This study presents a proof-of-concept chemiluminescence-based immunosensor for rapid and accurate measurement of cTnI, with the potential for online monitoring. The immunosensor incorporates a flow cell design and a sensitive complementary metal-oxide-semiconductor (CMOS) camera for optical readout. A microfluidic setup was established to enable selective and quasi-online determination of cTnI within ten minutes. The sensor was tested with recombinant cTnI in phosphate buffer, demonstrating measurements in the concentration range of 2–25 µg/L, with a limit of detection (LoD) of 0.6 µg/L (23 pmol/L) achieved using the optimized system. The immunosensor exhibited high selectivity, as no cross-reactivity was observed with other recombinant proteins such as cTnT and cTnC at a concentration of 16 µg/L. Measurements with diluted blood plasma and serum yielded an LoD of 60 µg/L (2.4 nmol/L) and 70 µg/L (2.9 nmol/L), respectively. This biosensor offers a promising approach for the rapid and sensitive detection of cTnI, contributing to the diagnosis and management of acute myocardial infarction and other cardiac vascular diseases.
N2 - Das kardiale Troponin I (cTnI) ist ein wichtiger Biomarker für die Diagnose von Herz-Kreislauf-Erkrankungen, einschließlich des akuten Myokardinfarkts (AMI). In dieser Studie wird ein auf Chemilumineszenz basierender Immunsensor für die schnelle und genaue Messung von cTnI vorgestellt, der das Potenzial für eine Online-Überwachung hat. Der Immunsensor besteht aus einer Durchflusszelle und einer empfindlichen CMOS-Kamera (Complementary Metal-Oxide-Semiconductor) zur optischen Detektion. Es wurde ein mikrofluidischer Aufbau entwickelt, der eine selektive und quasi Online-Bestimmung von cTnI innerhalb von zehn Minuten ermöglicht. Der Sensor wurde mit rekombinantem cTnI in Phosphatpuffer getestet und zeigte einen Messbereich von 2-25 µg/L, wobei mit dem optimierten System eine Nachweisgrenze (LoD) von 0,6 µg/L (23 pmol/L) erreicht wurde. Der Immunsensor zeigte eine hohe Selektivität, da keine Kreuzreaktivität mit anderen rekombinanten Proteinen wie cTnT und cTnC bei einer Konzentration von 16 µg/L beobachtet wurde. Messungen mit verdünntem Blutplasma und Serum ergaben einen LoD von 60 µg/L (2,4 nmol/L) bzw. 70 µg/L (2,9 nmol/L). Dieser Biosensor bietet einen vielversprechenden Ansatz für den schnellen und empfindlichen Nachweis von cTnI, der zur Diagnose und Behandlung des akuten Myokardinfarkts und anderer kardialer Gefäßerkrankungen beitragen kann.
KW - Acute myocardial infarction
KW - Heart attack
KW - Emergency
KW - Diagnosis
KW - Cardiac troponin
KW - Biomarker
KW - Immunosensor
KW - Biosensor
KW - Chemiluminescence
KW - Luminol
KW - Peroxidase
KW - Monoclonal antibodies
KW - Flow injection immunoassay
KW - Immunometric assay
KW - Immunometric biosensor
KW - Microfluidic system
KW - Monolithic column
KW - Online biosensor
PY - 2023
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-575471
DO - https://doi.org/10.3390/bios13040455
SN - 2079-6374
VL - 13
IS - 4
SP - 1
EP - 20
PB - MDPI
CY - Basel
AN - OPUS4-57547
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Peters, Stefan
A1 - Kunkel, Benny
A1 - Cakir, Cafer Tufan
A1 - Kabelitz, Anke
A1 - Witte, Steffen
A1 - Bernstein, Thomas
A1 - Bartling, Stephan
A1 - Radtke, Martin
A1 - Emmerling, Franziska
A1 - Abdel-Mageed, Ali Mohamed
A1 - Wohlrab, Sebastian
A1 - de Oliveira Guilherme Buzanich, Ana
T1 - Time-, space- and energy-resolved in situ characterization of catalysts by X-ray absorption spectroscopy
N2 - A novel setup for dispersive X-ray absorption spectroscopy (XAS) with simultaneous resolution of space, time and energy for in situ characterization of solid materials is demonstrated.
KW - Dispersive XAS
KW - Catalysis
KW - In situ
KW - Structure analysis
PY - 2023
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-584924
DO - https://doi.org/10.1039/d3cc03277a
SN - 1359-7345
SP - 1
EP - 4
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-58492
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - de Oliveira Guilherme Buzanich, Ana
A1 - Radtke, Martin
A1 - Yusenko, Kirill
A1 - Stawski, Tomasz
A1 - Kulow, Anicó
A1 - Cakir, Cafer Tufan
A1 - Röder, Bettina
A1 - Naese, Christoph
A1 - Britzke, Ralf
A1 - Sintschuk, Michael
A1 - Emmerling, Franziska
T1 - BAMline - A real-life sample materials research beamline
N2 - With increasing demand and environmental concerns, researchers are exploring new materials that can perform as well or better than traditional materials while reducing environmental impact. The BAMline, a real-life sample materials research beamline, provides unique insights into materials’ electronic and chemical structure at different time and length scales. The beamline specializes in x-ray absorption spectroscopy, x-ray fluorescence spectroscopy, and tomography experiments. This enables real-time optimization of material properties and performance for various applications, such as energy transfer, energy storage, catalysis, and corrosion resistance. This paper gives an overview of the analytical methods and sample environments of the BAMline, which cover non-destructive testing experiments in materials science, chemistry, biology, medicine, and cultural heritage. We also present our own synthesis methods, processes, and equipment developed specifically for the BAMline, and we give examples of synthesized materials and their potential applications. Finally, this article discusses the future perspectives of the BAMline and its potential for further advances in sustainable materials research.
KW - Extended X-ray absorption fine structure
KW - Energy storage
KW - Environmental impacts
KW - Nondestructive testing techniques
KW - X-ray fluorescence spectroscopy
KW - Corrosion
KW - Near edge X-ray absorption fine structure spectroscopy
KW - X-ray absorption spectroscopy
PY - 2023
DO - https://doi.org/10.1063/5.0157194
VL - 158
IS - 24
SP - 1
EP - 22
PB - AIP Publishing
AN - OPUS4-57824
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Karafiludis, Stephanos
A1 - Kochovski, Z.
A1 - Scoppola, E.
A1 - Retzmann, Anika
A1 - Hodoroaba, Vasile-Dan
A1 - ten Elshof, J. E.
A1 - Emmerling, Franziska
A1 - Stawski, Tomasz Maciej
T1 - Nonclassical Crystallization Pathway of Transition Metal Phosphate Compounds
N2 - Here, we elucidate nonclassical multistep crystallization pathways of transition metal phosphates from aqueous solutions. We followed precipitation processes of M-struvites, NH4MPO4·6H2O, and M-phosphate octahydrates, M3(PO4)2·8H2O, where M = Ni, Co, or NixCo1–x, by using in situ scattering and spectroscopy-based techniques, supported by elemental mass spectrometry analyses and advanced electron microscopy. Ni and Co phosphates crystallize via intermediate colloidal amorphous nanophases, which change their complex structures while agglomerating, condensing, and densifying throughout the extended reaction times. We reconstructed the three-dimensional morphology of these precursors by employing cryo-electron tomography (cryo-ET). We found that the complex interplay between metastable amorphous colloids and protocrystalline units determines the reaction pathways. Ultimately, the same crystalline structure, such as struvite, is formed. However, the multistep process stages vary in complexity and can last from a few minutes to several hours depending on the selected transition metal(s), their concentration, and the Ni/Co ratio.
KW - Non-classical crystallization theory
KW - Transition metals
KW - Phosphates
KW - Amorphous phases
KW - Intermediate phases
PY - 2023
DO - https://doi.org/10.1021/acs.chemmater.3c02346
SN - 1520-5002
VL - 35
IS - 24
SP - 10645
EP - 10657
PB - American Chemical Society (ACS)
CY - Washington D.C.
AN - OPUS4-59135
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Cakir, Cafer Tufan
A1 - Piotrowiak, T.
A1 - Reinholz, Uwe
A1 - Ludwig, A.
A1 - Emmerling, Franziska
A1 - Streli, C.
A1 - de Oliveira Guilherme Buzanich, Ana
A1 - Radtke, Martin
T1 - Exploring the Depths of Corrosion: A Novel GE-XANES Technique for Investigating Compositionally Complex Alloys
N2 - In this study, we propose the use of nondestructive, depth-resolved, element-specific characterization using grazing exit X-ray absorption near-edge structure spectroscopy (GE-XANES) to investigate the corrosion process in compositionally complex alloys (CCAs). By combining grazing exit X-ray fluorescence spectroscopy (GE-XRF) geometry and a pnCCD detector, we provide a scanning-free, nondestructive, depth-resolved analysis in a sub-micrometer depth range, which is especially relevant for layered materials, such as corroded CCAs. Our setup allows for spatial and energy-resolved measurements and directly extracts the desired fluorescence line, free from scattering events and other overlapping lines. We demonstrate the potential of our approach on a compositionally complex CrCoNi alloy and a layered reference sample with known composition and specific layer thickness. Our findings indicate that this new GE-XANES approach has exciting opportunities for studying surface catalysis and corrosion processes in real-world materials.
KW - Degradation mechanisms
KW - Grazin exit XANES
KW - Depth resolved XANES
KW - Compositional complex alloys
KW - Corrosion
PY - 2023
DO - https://doi.org/10.1021/acs.analchem.3c00404
VL - 95
SP - 4810
EP - 4818
PB - ACS Publications
AN - OPUS4-57823
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - GEN
A1 - Prinz, Carsten
A1 - Zimathies, Annett
A1 - Emmerling, Franziska
T1 - Experimantal raw data sets associated with certified reference material BAM-P116 (titanium dioxide) for comparison of nitrogen and argon sorption, available in the universal adsorption information format (AIF)
N2 - These data sets serve as models for calculating the specific surface area (BET method) using gas sorption in accordance with ISO 9277.
The present measurements were carried out with nitrogen at 77 Kelvin and argon at 87 Kelvin.
It is recommended to use the following requirements for the molecular cross-sectional area:
Nitrogen: 0.1620 nm²
Argon: 0.1420 nm²
Titanium dioxides certified with nitrogen sorption and additionally measured with argon for research purposes were used as sample material.
The resulting data sets are intended to serve as comparative data for own measurements and show the differences in sorption behaviour and evaluations between nitrogen and argon.
These data are stored in the universal AIF format (adsorption information file), which allows flexible use of the data.
KW - Physisorption
KW - Surface area
KW - AIF
KW - Argon
KW - Nitrogen
PY - 2023
DO - https://doi.org/10.5281/zenodo.10199628
PB - Zenodo
CY - Geneva
AN - OPUS4-59102
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Somasundaram, S. K.
A1 - de Oliveira Guilherme Buzanich, Ana
A1 - Emmerling, Franziska
A1 - Krishnan, S.
A1 - Senthilkumar, K.
A1 - Joseyphus, R.J.
T1 - New insights into pertinent Fe-complexes for the synthesis of iron via the instant polyol process
N2 - Chemically synthesized iron is in demand for biomedical applications due to its large saturation magnetization compared to iron oxides. The polyol process, suitable for obtaining Co and Ni particles and their alloys, is laborious in synthesizing Fe. The reaction yields iron oxides, and the reaction pathway remains unexplored. This study shows that a vicinal polyol, such as 1,2-propanediol, is suitable for obtaining Fe rather than 1,3-propanediol owing to the formation of a reducible Fe intermediate complex. X-ray absorption spectroscopy analysis reveals the ferric octahedral geometry and tetrahedral geometry in the ferrous state of the reaction intermediates in 1,2-propanediol and 1,3-propanediol, respectively. The final product obtained using a vicinal polyol is Fe with a γ-Fe2O3 shell, while the terminal polyol is favourable for Fe3O4. The distinct Fe–Fe and Fe–O bond lengths suggest the presence of a carboxylate group and a terminal alkoxide ligand in the intermediate of 1,2-propanediol. A large Fe–Fe bond distance suggests diiron complexes with bidentate carboxylate bridges. Prominent high-spin and low-spin states indicate the possibility of transition, which favors the reduction of iron ions in the reaction using 1,2-propanediol.
KW - XAS
KW - Nanoparticle
PY - 2023
DO - https://doi.org/10.1039/D3CP01969A
SN - 1463-9076
VL - 25
IS - 33
SP - 21970
EP - 21980
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-58073
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Gugin, Nikita
A1 - Villajos Collado, José Antonio
A1 - Dautain, O.
A1 - Maiwald, Michael
A1 - Emmerling, Franziska
T1 - Optimizing the Green Synthesis of ZIF-8 by Reactive Extrusion Using In Situ Raman Spectroscopy
N2 - We report the scale-up of a batch solid synthesis of zeolitic imidazolate framework-8 (ZIF-8) for reactive extrusion. The crystalline product forms in the extruder directly under the mixture of solid 2-methylimidazole and basic zinc carbonate in the presence of a catalytic amount of liquid. The process parameters such as temperature, liquid type, feeding rate, and linker excess were optimized using the setup specifically designed for in situ Raman spectroscopy. Highly crystalline ZIF-8 with a Brunauer–Emmett–Teller (BET) surface area of 1816 m2 g–1 was quantitatively prepared at mild temperature using a catalytic amount of ethanol and a small excess of the linker. Finally, we developed a simple and comprehensive approach to evaluating the environmental friendliness and scalability of metal–organic framework (MOF) syntheses in view of their large-scale production.
KW - Mechanochemistry
KW - In situ Raman
KW - Large-scale processing
KW - Metal−organic frameworks
KW - Twin-screw extrusion (TSE)
PY - 2023
DO - https://doi.org/10.1021/acssuschemeng.2c07509
SN - 2168-0485
VL - 11
IS - 13
SP - 5175
EP - 5183
PB - ACS Publications
AN - OPUS4-57366
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - CONF
A1 - Radtke, Martin
T1 - Insights into materials with hard x-rays: capabilities of the bamline
N2 - This contribution provides an overview of the BAMline synchrotron radiation beamline, which specializes in hard X-ray spectroscopy techniques for materials research. The BAMline offers X-ray absorption spectroscopy (XAS), x-ray fluorescence spectroscopy (XRF), and tomography to study materials' electronic structure, chemical composition, and structure. Key capabilities include standard and dispersive XAS for electronic structure, micro-XRF for elemental mapping, coded aperture imaging, and depth-resolved grazing exit XAS. The BAMline enables in situ characterization during materials synthesis and functions for energy, catalysis, corrosion, biology, and cultural heritage applications.
Ongoing developments like the implementation of machine learning techniques for experiment optimization and data analysis will be discussed. For instance, Bayesian optimization is being used to improve beamline alignment and scanning. An outlook to the future, where the BAMline will continue pioneering dynamic and multi-scale characterization, aided by advanced data science methods, to provide unique insights into materials research, will be given.
T2 - μ-XRF at Elettra 2.0: challenges and opportunities
CY - Trieste, Italy
DA - 11.09.2023
KW - Synchrotron
KW - XRF
KW - XANES
KW - Bayes
PY - 2023
AN - OPUS4-58607
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - CONF
A1 - Dalgic, Mete-Sungur
T1 - Lösemittelfreie Probenpräparation zur Untersuchung von Polymerblends mittels MALDI-TOF MS
N2 - Die Probenpräparation ist ein wichtiger Schritt für die Qualität der Massenspektren in MALDI-TOF MS. Es werden Polymerproben, die lösungsmittelbasiert und lösungsmittelfrei präpariert worden sind, verglichen. Dabei werden die Intensitätsverhältnisse von ternären Mischungen von PEG-, PS- und PMMA-Polymeren beachtet.
T2 - 28. Kolloquium - Massenspektrometrische Techniken zur Untersuchung synthetischer Polymere
CY - Berlin, Germany
DA - 14.05.2024
KW - Polymere
KW - Massenspektrometrie
KW - Probenpräparation
PY - 2024
AN - OPUS4-60032
LA - deu
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - CONF
A1 - Cakir, Cafer Tufan
T1 - Enhancing the Efficiency and Accessibility of Grazing Exit X-ray Absorption Spectroscopy for Corrosion and Layered Materials Analysis
N2 - In the field of materials science, there is a critical need for efficient and effective characterization techniques, especially in the investigation of corrosion processes of compositionally complex alloys (CCAs) or the analysis of layered structures. This talk presents an advanced approach that combines grazing-exit X-ray absorption near-edge structure spectroscopy (GE-XANES) with Bayesian optimization (BO) to significantly improve the efficiency of data acquisition while retaining the depth-resolved, element-specific analysis capabilities that are critical for studying these materials under ambient conditions. Using a non-destructive, scan-free GE-XANES setup coupled with a pnCCD detector and grazing exit X-ray fluorescence spectroscopy (GE-XRF) geometry, our method enables precise analysis at sub-micrometer depths without the need for high vacuum environments or extensive sample preparation. The integration of BO reduces experimental time by a factor of 50, overcoming the practical limitations of conventional GE-XANES and increasing its applicability in the study of surface catalysis and corrosion processes. We validate this optimized approach through comparative studies on a CrCoNi alloy and a reference layered sample, demonstrating its potential to revolutionize materials analysis by increasing both efficiency and accessibility.
T2 - Gesellschaft Deutscher Chemiker (GDCh)
CY - Clausthal-Zellerfeld, Germany
DA - 20.06.2024
KW - GEXRF
KW - GEXANE
KW - ML
PY - 2024
AN - OPUS4-61788
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Weidner, Steffen
A1 - Meyer, A.
A1 - Kricheldorf, H.
T1 - Transformation of poly(L-lactide) crystals composed of linear chains into crystals composed of cycles
N2 - A poly(L-lactide) with a trifluoroethyl ester end group and an average degree of polymerization (DP) of 50 was synthesized by ROP of L-lactide initiated with trifluoroethanol. Small-angle X-ray scattering (SAXS) in combination with differential scanning calorimetry (DSC) measurements revealed an average crystal thickness of 13 nm, corresponding to 45 repeat units. This suggests that most crystallites were formed by extended PLA chains, and both flat surfaces were covered by CF3 groups. The crystalline PLAs were annealed at 140 or 160 °C in the presence of two catalysts: tin(II) 2-ethylhexanoate, (SnOct2) or dibutyltin bis(pentafluorophenoxide) (BuSnPhF). The chemical reactions, such as polycondensation and cyclization, proceeded in the solid state and were monitored by matrix-assisted laser desorption/ionization time-offlight (MALDI TOF) mass spectrometry and gel permeation chromatography (GPC) measurements. Under optimal conditions a large fraction of linear chains was transformed into crystallites composed of extended cycles. Additionally, MALDI TOF MS analysis of GPC fractions from samples annealed for 28 or 42 days detected chain elongation of the linear species up to a factor of 20.
KW - Polylactide
KW - MALDI-TOF MS
KW - Crystalinity
KW - Transesterification
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-597250
DO - https://doi.org/10.1039/D3PY01370G
SN - 1759-9954
VL - 15
IS - 12
SP - 1173
EP - 1181
PB - Royal Society for Chemistry
AN - OPUS4-59725
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Kricheldorf, H.
A1 - Weidner, Steffen
A1 - Meyer, A.
T1 - About alcohol-initiated polymerization of glycolide and separate crystallization of cyclic and linear polyglycolides
N2 - Alcohol-initiated polymerizations of glycolide (GL) catalyzed by tin(II) 2-ethylhexanoate (SnOct2) were carried out in bulk with variation of GA/In ratio, temperature and time. Due to a rather strong competition of cyclization polyglycolide (PGA) free of cycles were never obtained. When the cyclic catalysts 2,2-dibutal-2-stanna − 1,3-dithiolane (DSTL) or 2-stanna 1,3-dioxo-4,5,6,7 bibenzepane (SnBiph) were used in combination with 1,4-butanediol the influence of cyclization was even stronger. Furthermore, the degrees of polymerization were higher than the GA/alcohol ratio due to rapid polycondensation in the solid state. At 160 °C or below, the matrixassisted laser desorption/ionization time-of-flight (MALDI-TOF) mass spectra indicated separate crystallization of low molar mass cyclic and linear PGAs from the same reaction mixture (also observed for poly(L-lactide)s).
KW - MALDI TOF MS
KW - Polyglycolide
KW - Ring opening polymerization
KW - Cyclization
KW - Crystallization
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-607282
DO - https://doi.org/10.1016/j.polymer.2024.127440
SN - 0032-3861
VL - 309
SP - 1
EP - 9
PB - Elsevier Ltd.
AN - OPUS4-60728
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Weidner, Steffen
A1 - Scheliga, Felix
A1 - Kricheldorf, Hans R.
T1 - Polycondensation, Cyclization and Disproportionation of Solid Poly(L-lactide) Trifluoroethyl Esters and the Simultaneous Formation of Extended Chain Crystals and Extended Ring Crystals
N2 - Two poly(L-lactide)s (PLAs) with a degree of polymerization (DP) of 20 or 100 were prepared by trifluoroethanol-initiated ring-opening polymerization (ROP) catalyzed by tin(II) 2-ethyl hexanoate (SnOct2). These PLAs were annealed at 140 ◦C or at 160 ◦C in the presence of SnOct2, and the changes in topology and molecular weight distribution (MWD) were monitored by matrix-assisted laser desorption/ionization time-of flight (MALDI TOF) mass spectrometry and gel permeation chromatography (GPC). For the PLA with a DP 20, the main reaction was polycondensation combined with higher dispersities. In the case of the DP 100, PLA polycondensation was combined with disproportionation and the formation of a new MWD maximum around m/z 3500. In addition, extensive cyclization occurred, and the resulting cyclic PLAs crystallized separately from the linear chains in the form of extended ring crystals. These results also suggest that both extended chain and extended ring crystals posses the same crystal thickness as a result of thermodynamically controlled transesterification in the solid state.
KW - Polycondensation
KW - MALDI
KW - Polylactide
KW - Cyclization
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-616441
DO - https://doi.org/10.1016/j.polymer.2024.127800
VL - 315
SP - 1
EP - 9
PB - Elsevier Ltd.
AN - OPUS4-61644
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Kricheldorf, Hans R.
A1 - Weidner, Steffen
A1 - Meyer, A.
T1 - About Polycondensation, Disproportionation, and Cyclization of Acetylated Poly(L-Lactide) Esters
N2 - L-lactide (LA) is polymerized with ethyl L-lactate or trifluoroethanol as initiators (LA/In = 30/1), and the resulting poly(L-lactide) esters are acetylated with acetic anhydride. The acetylated PLA esters are mixed with SnOct2, dibutyltin bis(4-chlorophenoxide), or dibutyltin bis(pentafluorophenoxide) in solution and crystallized at 120 °C. The doped crystals are annealed at 140 °C or at 160 °C for 7, 14, and 28 days, and the chemical modifications that occurred in the solid state are monitored by matrix-assisted laser desorption/ionization time-of-flight (MALDI TOF) mass spectrometry, gel permeation chromatography (GPC), and differential scanning calorimetry (DSC) measurements. All catalysts promoted polycondensation, while no significant formation of cycles is observed. However, in the presence of SnOct2, disproportionation of chains occurred upon annealing at 120 or 140 °C, and crystallites consisting of extended chains with Mn values ≈3500 – 3600 and low dispersities (Ð < 1.5) are formed.
KW - MALDI-TOF MS
KW - Polycondensation
KW - Polylactides
KW - Transesterifcation
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-630349
DO - https://doi.org/10.1002/macp.202400175
SN - 1521-3935
VL - 225
IS - 19
PB - Wiley VHC-Verlag
AN - OPUS4-63034
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Trimpin, Sarah
A1 - Yenchick, Frank S.
A1 - Lee, Chuping
A1 - Hoang, Khoa
A1 - Pophristic, Milan
A1 - Karki, Santosh
A1 - Marshall, Darrell D.
A1 - Lu, I-Chung
A1 - Lutomski, Corinne A.
A1 - El-Baba, Tarick J.
A1 - Wang, Beixi
A1 - Pagnotti, Vincent S.
A1 - Meher, Anil K.
A1 - Chakrabarty, Shubhashis
A1 - Imperial, Lorelei F.
A1 - Madarshahian, Sara
A1 - Richards, Alicia L.
A1 - Lietz, Christopher B.
A1 - Moreno-Pedraza, Abigail
A1 - Leach, Samantha M.
A1 - Gibson, Stephen C.
A1 - Elia, Efstathios A.
A1 - Thawoos, Shameemah M.
A1 - Woodall, Daniel W.
A1 - Jarois, Dean R.
A1 - Davis, Eric T.J.
A1 - Liao, Guochao
A1 - Muthunayake, Nisansala S.
A1 - Redding, McKenna J.
A1 - Reynolds, Christian A.
A1 - Anthony, Thilani M.
A1 - Vithanarachchi, Sashiprabha M.
A1 - DeMent, Paul
A1 - Adewale, Adeleye O.
A1 - Yan, Lu
A1 - Wager-Miller, James
A1 - Ahn, Young-Hoon
A1 - Sanderson, Thomas H.
A1 - Przyklenk, Karin
A1 - Greenberg, Miriam L.
A1 - Suits, Arthur G.
A1 - Allen, Matthew J.
A1 - Narayan, Srinivas B.
A1 - Caruso, Joseph A.
A1 - Stemmer, Paul M.
A1 - Nguyen, Hien M.
A1 - Weidner, Steffen
A1 - Rackers, Kevin J.
A1 - Djuric, Ana
A1 - Shulaev, Vladimir
A1 - Hendrickson, Tamara L.
A1 - Chow, Christine S.
A1 - Pflum, Mary Kay H.
A1 - Grayson, Scott M.
A1 - Lobodin, Vladislav V.
A1 - Guo, Zhongwu
A1 - Ni, Chi-Kung
A1 - Walker, J. Michael
A1 - Mackie, Ken
A1 - Inutan, Ellen D.
A1 - McEwen, Charles N.
T1 - New Processes for Ionizing Nonvolatile Compounds in Mass Spectrometry: The Road of Discovery to Current State-of-the-Art
N2 - This Perspective covers discovery and mechanistic aspects aswell as initial applications of novel ionization processes for use in massspectrometry that guided us in a series of subsequent discoveries, instrumentdevelopments, and commercialization. Vacuum matrix-assisted ionization onan intermediate pressure matrix-assisted laser desorption/ionization sourcewithout the use of a laser, high voltages, or any other added energy wassimply unbelievable, at first. Individually and as a whole, the variousdiscoveries and inventions started to paint, inter alia, an exciting new pictureand outlook in mass spectrometry from which key developments grew thatwere at the time unimaginable, and continue to surprise us in its simplisticpreeminence. We, and others, have demonstrated exceptional analyticalutility. Our current research is focused on how best to understand, improve, and use these novel ionization processes throughdedicated platforms and source developments. These ionization processes convert volatile and nonvolatile compounds from solid orliquid matrixes into gas-phase ions for analysis by mass spectrometry using, e.g., mass-selected fragmentation and ion mobilityspectrometry to provide accurate, and sometimes improved, mass and drift time resolution. The combination of research anddiscoveries demonstrated multiple advantages of the new ionization processes and established the basis of the successes that lead tothe Biemann Medal and this Perspective. How the new ionization processes relate to traditional ionization is also presented, as wellas how these technologies can be utilized in tandem through instrument modification and implementation to increase coverage ofcomplex materials through complementary strengths.
KW - Mass spectrometry
PY - 2024
DO - https://doi.org/10.1021/jasms.3c00122
SN - 1879-1123
VL - 35
IS - 12
SP - 2753
EP - 2784
PB - American Chemical Society (ACS)
AN - OPUS4-61417
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Dalgic, Mete-Sungur
A1 - Weidner, Steffen
T1 - Solvent-free sample preparation for matrix-assisted laserdesorption/ionization time-of-flight mass spectrometry ofpolymer blends
N2 - Solvent-free sample preparation offers some advantages over solvent-based techniques, such as improved accuracy, reproducibility and sensitivity, for matrix-assisted laser desorption/ionization (MALDI) analysis. However, little or no information is available on the application of solvent-free techniques for the MALDI analysis of polymer blends. Solvent-free sample preparation by ball milling was applied with varying sample-to-matrix ratios for MALDI time-of-flight mass spectrometry analysis of various polymers, including polystyrenes, poly(methyl methacrylate)s and poly(ethylene glycol)s. The peak intensity ratios were compared with those obtained after using the conventional dried droplet sample preparation method. In addition, solvent-assisted milling was also applied to improve sample homogeneities.
Depending on the sample preparation method used, different peak intensity ratios were found, showing varying degrees of suppression of the signal intensities of higher mass polymers. Ball milling for up to 30 min was required to achieve constant intensity ratios indicating homogeneous mixtures. The use of wet-assisted grinding to improve the homogeneity of the blends was found to be disadvantageous as it caused partial degradation and mass-dependent segregation of the polymers in the vials.The results clearly show that solvent-free sample preparation must be carefully considered when applied to synthetic polymer blends, as it may cause additional problems with regard to homogeneity and stability of the blends.
KW - MALDI TOF MS
KW - Sample preparation
KW - Polymer blends
KW - Solvent-free
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-598570
DO - https://doi.org/10.1002/rcm.9756
SN - 0951-4198
VL - 38
IS - 12
SP - 1
EP - 9
PB - Wiley online library
AN - OPUS4-59857
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Grimmer, Christoph
A1 - Richter, Matthias
A1 - Neuhaus, T.
A1 - Prinz, Carsten
A1 - Strzelczyk, Rebecca Skadi
A1 - Colakoglu, Irem
A1 - Horn, Wolfgang
T1 - Towards a multi-VOC emission reference material with temporally constant emission profile for QA/QC of materials emission testing procedures
N2 - Emission reference materials (ERMs) are sought after to further control and improve indoor air quality. The impregnation of porous materials with volatile organic compounds (VOCs) is a promising approach to produce ERMs. Different VOCs were used to impregnate various porous materials (mainly zeolites, activated carbons and a metal organic framework). The influence of different methodological parameters and material properties were studied to optimize the impregnation procedure and to find the best material/VOC combination. The impregnation procedure remains quite irreproducible, nevertheless, very good ERM candidates were identified. Two materials (zeolite 4 and AC 1 impregnated with n-hexadecane) showed a very stable emission over 14 days (<10 % change). Another material (AC 1 impregnated with toluene) showed a declining emission profile but with a very good in-batch reproducibility and a storage stability of up to 12 months.
KW - Emission reference material
KW - Porous materials
KW - Indoor air quality
KW - Emission test chamber
KW - CO2 assisted impregnation
KW - EN 16516
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-612238
DO - https://doi.org/10.1016/j.chemosphere.2024.143437
SN - 1879-1298
VL - 366
SP - 1
EP - 8
PB - Elsevier
AN - OPUS4-61223
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Valentim Gelamo, Rogério
A1 - Bueno Leite, Natália
A1 - de Sousa Amadeu, Nader
A1 - Reis Pedreira Muniz Tavares, Michel
A1 - Oberschmidt, Dirk
A1 - Klemm, Sophie
A1 - Fleck, Claudia
A1 - Cakir, Cafer-Tufan
A1 - Radtke, Martin
A1 - Aparecido Moreto, Jéferson
T1 - Exploring the Nb2O5 coating deposited on the Ti-6Al-4V alloy by a novel GE-XANES technique and nanoindentation load-depth
N2 - This research group has been demonstrating the significant advantages of using Nb2O5 coatings for functionalizing titanium, aluminium, and stainless steels. Regarding the biomedical sector and considering Ti-6Al-4V alloy, the reactive sputtering technique improved the cell viability, the osteogenic performance of cells involved in the osseointegration process as well as the ability to delay bacterial proliferation. The characteristics of the Nb2O5 coatings were assessed before by using standard methods, which provide information only a few tens of nanometers depth. Given that the Nb2O5 coating fabricated in this work exhibits a thickness of approximately 300 nm, the GE-XANES technique emerges as the most suitable method for this analysis. Additional information was provided with the aid of nanoindentation load-depth (P-h) curves. GE-XANES results indicated the formation of a homogeneous layer of Nb2O5 coating on the Ti-6Al-4V surfaces. The deposition process improved the surface hardness of the Ti-6Al-4V alloy (4.38 GPa versus 5.62 GPa) considering the 2 mN load.
KW - BAMline
KW - GE-XANES
KW - Synchrotron
PY - 2024
DO - https://doi.org/10.1016/j.matlet.2023.135584
SN - 0167-577X
VL - 355
SP - 1
EP - 4
PB - Elsevier B.V.
AN - OPUS4-60835
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - CONF
A1 - Radtke, Martin
T1 - ChatGPT and EPICS: LLM-Enhanced Control Systems for Synchrotron Beamlines
N2 - The document highlights ChatGPT-EPICS integration for synchrotron beamline automation, employing tools like motor records, PV naming systems, and LLM inference. It evaluates efficiency and challenges in implementing automated motor optimization and handling EPICS controls.
T2 - BESSY science seminar
CY - Online meeting
DA - 22.11.2024
KW - Chatgpt
KW - EPICS
KW - BAMline
PY - 2024
AN - OPUS4-61896
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - CONF
A1 - Radtke, Martin
T1 - From Egypt to Hiddensee – Analysis of Gold with Synchrotron Radiation V
N2 - Gold is one of the seven metals already known in antiquity and was used from time immemorial as a medium of exchange and for the production of jewelry because of its luster and rarity. In addition, it is easy to work and largely resistant to chemical influences. Investigations of gold using synchrotron radiation excited X-ray fluorescence analysis are non-destructive and provide information about the chemical elements present in the sample under investigation. The investigations presented here at BAMline focus on questions such as the origin, manufacturing process, and association of gold findings. The different questions are explained by a number of examples ranging from the Viking treasure from Hiddensee to the Nebra Sky Disk and finds from Egypt. The find from Bernstorf is discussed in detail. A Bayesian treatment of the authenticity is shown.
T2 - Ringvorlesung Einführung in die Archäometrie
CY - Berlin, Germany
DA - 01.11.2024
KW - Gold
KW - Synchrotron
KW - XRF
KW - BAMline
KW - Bayes
PY - 2024
AN - OPUS4-61699
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - CONF
A1 - Radtke, Martin
T1 - Decoding the Elemental Fingerprints of Ancient Gold: A Synchrotron-based Approach
N2 - This contribution focuses on the application of synchrotron radiation X-ray fluorescence (SR XRF) for the analysis of ancient gold objects at the BAMline, showcasing several noteworthy examples. One prominent artifact is the Sky Disc of Nebra, which presented a relatively straightforward question to be addressed: Do the gold inlays belong together, and can we glean insights about their origin? In contrast, the analysis of the Bernstorf gold, an alleged Bronze Age treasure composed of exceptionally pure gold, posed a more intricate challenge. The debate surrounding its authenticity prompted an in-depth investigation utilizing SR XRF with different experimental conditions. This approach, involving the analysis of trace elements, played a pivotal role in elucidating the nature and age of the gold, offering valuable insights into its production Platinum emerges as a crucial trace element for gold analysis, given its typically low concentration in gold artifacts, often in the range of a few parts per million (ppm). Accurately measuring Platinum in the presence of overlapping emission lines from gold is arduous. To overcome this challenge, BAMline developed a wavelength dispersive set-up known as D2XRF, employing a pixelated energy-dispersive X-ray detector (pnCCD). This innovative approach enables the resolution of overlapping emission lines, leading to a remarkable detection limit of 1 ppm for Platinum in gold samples. Furthermore, the application of the pnCCD for imaging element distributions on a Phoenician ivory artifact will be showcased. This technique allows for the visualization and mapping of various elements, which opens the possibility to reconstruct the original appearance. The comprehensive analysis of ancient gold artifacts at BAMline has provided valuable insights into the craftsmanship, trade, and technological advancements of ancient civilizations. By unraveling the complex stories these artifacts carry, our studies contributed significantly to the fields of archaeology, history, and materials science. It underscores the importance of interdisciplinary approaches in piecing together the puzzle of human history, revealing the interconnectedness of cultures through the lens of non-destructive analysis.
T2 - Denver X-ray Conference 2024
CY - Denver, CO, USA
DA - 04.08.2024
KW - Gold
KW - Synchrotron
KW - XRF
KW - BAMline
PY - 2024
AN - OPUS4-61701
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Leidigkeit, Carolin
A1 - Shokr, Mohammad
A1 - Tosson, Amir
A1 - Cakir, Cafer Tufan
A1 - Radtke, Martin
A1 - Pietsch, Ullrich
A1 - Christ, Hans-Jürgen
T1 - Using Energy-Dispersive Laue Diffraction to Study Dislocation Arrangements in Materials Showing Wavy and Planar Slip Behavior
N2 - The present work shows an approach to monitor the evolution of the dislocation arrangement of a metallic material caused by cyclic plastic strain using white X-ray radiation in combination with an energy-dispersive detector. The method is demonstrated by single-shot experiments performed on polycrystalline nickel and α-brass, representing the pure wavy and the pure planar dislocation slip behavior. To correlate the resulting diffraction patterns with various dislocation arrangements of both metals, fatigue tests were carried out up to certain numbers of cycles and at predetermined plastic strain amplitudes. The differences in dislocation microstructure and internal stress distributions give rise to an appreciable change in the peak shape of Laue reflections, leading to unique characteristics in the respective diffraction patterns. Nickel reflections are elongated due to the high amount of cell structures leading to bending and misorientation of the lattice, whereas the present stacking faults in α-brass result in powder-like diffraction.
KW - Slip behavior
KW - Energy-Dispersive
KW - Laue Diffraction
KW - Dislocation
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-637964
DO - https://doi.org/10.1111/ffe.14535
SN - 1460-2695
VL - 48
IS - 3
SP - 1341
EP - 1351
PB - Wiley
AN - OPUS4-63796
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - CONF
A1 - Radtke, Martin
T1 - ChatGPT and EPICS: LLM-Enhanced Control Systems for Synchrotron Beamlines
N2 - The BAMline at BESSY II represents a hard X-ray spectroscopy facility enabling non-destructive analysis across diverse research areas like materials science, chemistry, biology, and cultural heritage studies. As a multipurpose beamline serving users from various disciplines, it underscores the necessity of adaptable and efficient control systems to maximize beamline utilization and scientific output.
In this contribution, we detail the innovative integration of ChatGPT , OpenAI’s state-of-the-art Large Language Model (LLM), with the Experimental Physics and Industrial Control System (EPICS) which underpins the operational framework of the BAMline. This integration leverages the advanced natural language processing (NLP) capabilities of ChatGPT, presenting a revolutionary approach to beamline control that markedly simplifies user interaction. Through this, we facilitate a user-friendly pathway to executing complex experimental setups, eliminating the barrier imposed by conventional scripting languages and the often-challenging graphical user interfaces. This innovation promises to significantly streamline experimental workflows, thereby enhancing the efficiency of scientific research conducted at the beamline.
Further enhancing this user-centric approach, we introduce an advanced graphical user interface (GUI) application. This novel application seamlessly melds the LLM’s NLP capabilities with EPICS, thereby enabling researchers to articulate experimental requirements through simple textual or voice commands. This interface interprets these commands to manipulate various beamline components, including but not limited to the Double Crystal Monochromator (DCM), Double Multilayer Monochromator (DMM), as well as various filters and slits. By parsing user input, extracting pertinent parameters, and generating a structured JSON object that reflects the desired device positions and experimental settings, the GUI application bridges the gap between complex control commands and intuitive user interactions. This advancement not only lowers the entry threshold for new users but also streamlines the operational workflow for experienced researchers.
Looking ahead, we aim to extend the system to cover the entire experimental cycle, from setup to data analysis. Using LLMs, one could translate plain-language experiment descriptions into precise operational commands, revolutionizing the research process and making advanced scientific exploration more accessible to a wider community.
T2 - European X-ray Spectrometry Conference
CY - Athens, Greece
DA - 24.06.2024
KW - EPICS
KW - ChatGPT
KW - BAMline
KW - Synchrotron
PY - 2024
AN - OPUS4-61702
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - CONF
A1 - Radtke, Martin
T1 - Vergangenheit verifiziert: Datierung und Authentizität mittels Bayes’scher Methoden
N2 - In der Archäologie ist die präzise Datierung von Funden und die Verifikation ihrer Authentizität von entscheidender Bedeutung, um Erkenntnisse über vergangene Zivilisationen zu gewinnen. Während traditionelle Methoden wie die Radiokarbon-Datierung bereits seit Jahrzehnten etabliert sind, hat die Anwendung der Bayes’schen Statistik in den letzten Jahren an Bedeutung gewonnen. Dieser Ansatz erlaubt es, vorhandene Unsicherheiten in archäologischen Daten systematisch zu berücksichtigen und bietet somit eine leistungsfähige Ergänzung zu herkömmlichen Methoden.
Die Bayes’sche Theorie basiert auf der Aktualisierung von Wahrscheinlichkeiten anhand neuer Daten. Dies ist besonders nützlich in der Archäologie, wo neue Funde oft bestehende Theorien und Annahmen in Frage stellen. Durch die Kombination von Prior-Wissen mit neuen Daten ermöglicht die Bayes'sche Methode eine adaptive und flexible Datierung und Verifizierung.
Ein Beispiel für die Anwendung dieser Methode ist die Radiokarbon-Datierung. Während die traditionelle Radiokarbon-Datierung einen geschätzten Zeitraum bietet, kann die Bayes'sche Analyse dazu verwendet werden, die Unsicherheit dieses Zeitraums zu quantifizieren und zu verfeinern. Dies ist besonders wertvoll bei der Datierung von Artefakten aus Zeiträumen, in denen mehrere historische Ereignisse stattfanden.
Zudem ist die Bayes'sche Methode auch bei der Überprüfung der Authentizität von Funden nützlich. Durch die Kombination verschiedener Datenquellen, wie z.B. Inschriften, Materialanalysen und Kontextinformationen, können Archäologen die Wahrscheinlichkeit der Echtheit eines Artefakts bestimmen.
Trotz ihrer Stärken ist die Anwendung der Bayes’schen Statistik in der Archäologie nicht ohne Herausforderungen. Die Wahl der Prior-Wahrscheinlichkeit kann subjektiv sein und die Methode erfordert eine sorgfältige Überlegung und Expertise.
Die Bayes’sche Methode in der Archäologie ein leistungsfähiges Werkzeug, um Datierungen zu verfeinern und die Authentizität von Funden zu überprüfen. Während traditionelle Methoden weiterhin eine zentrale Rolle spielen, ermöglicht der Bayes’sche Ansatz eine nuanciertere und adaptivere Analyse, die das Potential hat, unser Verständnis der Vergangenheit zu vertiefen.
T2 - NAHM workshop
CY - Bonn, Germany
DA - 18.10.2023
KW - Bayes
KW - Bernstorf
KW - Gold
KW - Datierung
KW - Herkunft
KW - Suchtheorie
PY - 2024
AN - OPUS4-61705
LA - deu
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - CONF
A1 - Radtke, Martin
T1 - ChatGPT and EPICS: LLM-Enhanced Control Systems for Synchrotron Beamlines
N2 - The BAMlineat BESSY II represents a hard X-ray spectroscopy facility enabling non-destructive analysis across diverse research areas like materials science, chemistry, biology, and cultural heritage studies. As a multipurpose beamline serving users from various disciplines, it underscores the necessity of adaptable and efficient control systems to maximize beamline utilization and scientific output.
In this contribution, we detail the innovative integration of ChatGPT, OpenAI’s state-of-the-art Large Language Model (LLM), with the Experimental Physics and Industrial Control System (EPICS) which underpins the operational framework of the BAMline. This integration leverages the advanced natural language processing (NLP) capabilities of ChatGPT, presenting a revolutionary approach to beamline control that markedly simplifies user interaction. Through this, we facilitate a user-friendly pathway to executing complex experimental setups, eliminating the barrier imposed by conventional scripting languages and the often-challenging graphical user interfaces. This innovation promises to significantly streamline experimental workflows, thereby enhancing the efficiency of scientific research conducted at the beamline.
Further enhancing this user-centric approach, we introduce an advanced graphical user interface (GUI) application. This novel application seamlessly melds the LLM’s NLP capabilities with EPICS, thereby enabling researchers to articulate experimental requirements through simple textual or voice commands. This interface interprets these commands to manipulate various beamline components, including but not limited to the Double Crystal Monochromator (DCM), Double Multilayer Monochromator (DMM), as well as various filters and slits. By parsing user input, extracting pertinent parameters, and generating a structured JSON object that reflects the desired device positions and experimental settings, the GUI application bridges the gap between complex control commands and intuitive user interactions. This advancement not only lowers the entry threshold for new users but also streamlines the operational workflow for experienced researchers.
Looking ahead, we aim to extend the system to cover the entire experimental cycle, from setup to data analysis. Using LLMs, one could translate plain-language experiment descriptions into precise operational commands, revolutionizing the research process and making advanced scientific exploration more accessible to a wider community.
T2 - International Conference on Synchrotron Radiation Instrumentation (SRI)
CY - Hamburg, Germany
DA - 26.08.2024
KW - Chatgpt
KW - EPICS
KW - BAMline
KW - Synchrotron
PY - 2024
AN - OPUS4-61700
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - CONF
A1 - Radtke, Martin
T1 - Getting more efficient – The use of Bayesian optimization and Gaussian processes at the BAMline
N2 - The BAMline, a beamline for material science research at BESSY II, has been operated by the Bundesanstalt für Materialforschung und -prüfung for over two decades. In the last few years, Bayesian optimization (BO) with Gaussian processes (GP) has been introduced as a transformative method in this setting. This contribution highlights the integration and impact of BO and GP in refining BAMline operations.
We will explore the impact of integrating Bayesian methods, especially when combined with Gaussian processes, on the operational efficiency of the BAMline. Our discussion commences with an overview of the fundamental concepts of active learning and optimization. This is followed by an in-depth analysis of specific case studies, drawing on our direct experience with these innovative methods.
For this our focus is on three key applications:
Alignment of Optical Elements (DCM and DMM): The implementation of
Bayesian optimization using Gaussian processes has revolutionized the
alignment process for the Double Crystal Monochromator (DCM) and the
Double Multilayer Monochromator (DMM). This approach greatly reduced
manual effort and enhanced the efficiency and effectiveness of the
alignment procedure.
Optimal Spot Selection for Spatial Mapping in XRF Studies: In X-ray
fluorescence (XRF) experiments, determining the most informative
sampling spots is crucial. The introduction of BO, informed by GP,
has significantly improved the selection process, especially in large
or heterogeneous samples. This methodology ensures maximum
information gain, optimizing the balance between comprehensive
mapping and resource management.
Selection of Optimal Energies for XANES Measurements in GEXANES
Geometry: In the specific context of X-ray Absorption Near Edge
Structure (XANES) studies using Grazing Exit (GEXANES) geometry, the
Bayesian approach with Gaussian processes is now utilized to identify
the most effective energy settings. This results in detailed spectral
data acquired in a much shorter time.
We also address challenges and limitations encountered during implementation. Additionally, the versatility of this approach in addressing a range of different research questions will be demonstrated.
T2 - Machine Learning Conference for X-Ray and Neutron-Based Experiments
CY - Garching bei München, Germany
DA - 08.04.2024
KW - BAMline
KW - Synchrotron
KW - XRF
KW - Bayes
PY - 2024
AN - OPUS4-61703
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - CONF
A1 - Radtke, Martin
T1 - Machine learning - Examples from BAM Line
N2 - This talk explores applications of artificial intelligence in the field of spectroscopy, with a special focus on research conducted at BAMline. We begin with an overview of synchrotron radiation and its unique capabilities in material analysis. The first part of the talk will cover the integration of AI algorithms in quantifying X-ray fluorescence measurements, providing enhanced precision and efficiency in data analysis. Following this, we will examine the role of language models in spectroscopic research, showcasing how these tools can facilitate the control of complex experimental set-ups
T2 - Analytical Academy
CY - Berlin, Germany
DA - 12.11.2024
KW - ChatGPT
KW - Neural networks
KW - XRF
KW - Synchrotron
KW - BAMline
PY - 2024
AN - OPUS4-61698
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Dobosy, Péter
A1 - Nguyen, Hoang Thi Phuong
A1 - Záray, Gyula
A1 - Streli, Christina
A1 - Ingerle, Dieter
A1 - Ziegler, Philipp
A1 - Radtke, Martin
A1 - de Oliveira Guilherme Buzanich, Ana
A1 - Endrédi, Anett
A1 - Fodor, Ferenc
T1 - Effect of iodine species on biofortification of iodine in cabbage plants cultivated in hydroponic cultures
N2 - Iodine is an essential trace element in the human diet because it is involved in the synthesis of thyroid hormones. Iodine deficiency affects over 2.2 billion people worldwide, making it a significant challenge to find plant-based sources of iodine that meet the recommended daily intake of this trace element. In this study, cabbage plants were cultivated in a hydroponic system containing iodine at concentrations ranging from 0.01 to 1.0 mg/L in the form of potassium iodide or potassium iodate. During the experiments, plant physiological parameters, biomass production, and concentration changes of iodine and selected microelements in different plant parts were investigated. In addition, the oxidation state of the accumulated iodine in root samples was determined. Results showed that iodine addition had no effect on photosynthetic efficiency and chlorophyll content. Iodide treatment did not considerably stimulate biomass production but iodate treatment increased it at concentrations less than 0.5 mg/L. Increasing iodine concentrations in the nutrient solutions increased iodine content in all plant parts; however, the iodide treatment was 2–7 times more efficient than the iodate treatment. It was concluded, that iodide addition was more favourable on the target element accumulation, however, it should be highlighted that application of this chemical form in nutrient solution decreased the concetrations of selected micoelement concentration comparing with the control plants. It was established that iodate was reduced to iodide during its uptake in cabbage roots, which means that independently from the oxidation number of iodine (+ 5, − 1) applied in the nutrient solutions, the reduced form of target element was transported to the aerial and edible tissues.
KW - BAMline
KW - XANES
KW - Synchrotron
KW - Lodine
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-608330
DO - https://doi.org/10.1038/s41598-024-66575-z
VL - 14
IS - 1
SP - 1
EP - 12
PB - Springer Science and Business Media LLC
AN - OPUS4-60833
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Huang, Junhao
A1 - Klahn, Marcus
A1 - Tian, Xinxin
A1 - Bartling, Stephan
A1 - Zimina, Anna
A1 - Radtke, Martin
A1 - Rockstroh, Nils
A1 - Naliwajko, Pawel
A1 - Steinfeldt, Norbert
A1 - Peppel, Tim
A1 - Grunwaldt, Jan‐Dierk
A1 - Logsdail, Andrew J.
A1 - Jiao, Haijun
A1 - Strunk, Jennifer
T1 - Fundamental Structural and Electronic Understanding of Palladium Catalysts on Nitride and Oxide Supports
N2 - The nature of the support can fundamentally affect the function of a heterogeneous catalyst. For the novel type of isolated metal atom catalysts, sometimes referred to as single‐atom catalysts, systematic correlations are still rare. Here, we report a general finding that Pd on nitride supports (non‐metal and metal nitride) features a higher oxidation state compared to that on oxide supports (non‐metal and metal oxide). Through thorough oxidation state investigations by X‐ray absorption spectroscopy (XAS), X‐ray photoelectron spectroscopy (XPS), CO‐DRIFTS, and density functional theory (DFT) coupled with Bader charge analysis, it is found that Pd atoms prefer to interact with surface hydroxyl group to form a Pd(OH)x species on oxide supports, while on nitride supports, Pd atoms incorporate into the surface structure in the form of Pd−N bonds. Moreover, a correlation was built between the formal oxidation state and computational Bader charge, based on the periodic trend in electronegativity.
KW - BAmline
KW - XANES
KW - Catalyst
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-608341
DO - https://doi.org/10.1002/anie.202400174
SN - 1433-7851
VL - 63
IS - 20
SP - 1
EP - 9
PB - Wiley
AN - OPUS4-60834
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Peters, Stefan
A1 - Bartling, Stephan
A1 - Parlinska-Wojtan, Magdalena
A1 - Wotzka, Alexander
A1 - de Oliveira Guilherme Buzanich, Ana
A1 - Wohlrab, Sebastian
A1 - Abdel-Mageed, Ali M.
T1 - Stabilization of intermediate Mo oxidation states by Nb doping enhancing methane aromatization on Mo/HZSM-5 catalysts
N2 - The dehydroaromatization of methane is a promising process to produce aromatics and ultra-pure hydrogen. Increased yields and stability of Mo/HZSM-5 against irreversible deactivation were achieved via a redox interaction by doping with otherwise inert Nb.
KW - General Materials Science
KW - Sustainability and the Environment
KW - General Chemistry
KW - Renewable Energy
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-597670
DO - https://doi.org/10.1039/D3TA07532J
SN - 2050-7488
SP - 1
EP - 16
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-59767
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Senges, Gene
A1 - de Oliveira Guilherme Buzanich, Ana
A1 - Lindič, Tilen
A1 - Gully, Tyler A.
A1 - Winter, Marlon
A1 - Radtke, Martin
A1 - Röder, Bettina
A1 - Steinhauer, Simon
A1 - Paulus, Beate
A1 - Emmerling, Franziska
A1 - Riedel, Sebastian
T1 - Unravelling highly oxidized nickel centers in the anodic black film formed during the Simons process by in situ X-ray absorption near edge structure spectroscopy
N2 - The electrofluorination after Simons has been used for the last century to produce everyday life materials. An in situ XANES investigation of the controversially debated black film apparent in the Simons process revealed high-valent nickel centers.
KW - Synchrotron
KW - BAMline
KW - XANES
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-608366
DO - https://doi.org/10.1039/d3sc06081k
SN - 2041-6520
VL - 15
IS - 12
SP - 4504
EP - 4509
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-60836
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Meyer, Andreas
A1 - Weidner, Steffen
A1 - Kricheldorf, Hans R.
T1 - Star-shaped poly(l-lactide)s based on pentaerythritol: About crystallization and polycondensation plus disproportionation and ring formation in the solid state
N2 - Star-shaped poly( L-lactide)s (s-PLAs), were prepared by ring-opening polymerization of with pentaerythritol and catalyzed by tin(II) 2-ethylhyexanoate (SnOct out in bulk at either 120 ◦ C or 160 ◦ L-lactide (LA) initiated 2 ). Two small series of ROPs were carried C with variation of the LA/initiator ratio. Matrix-assisted laser desorption/ ionization time-of-flight (MALDI-TOF) mass spectra revealed traces of cycles in 120 ◦ C samples only at low initiator/catalyst ratios. In contrast, higher fractions of cycles were detected in samples prepared at 160 C, suggesting a "back-biting" origin. The influence of arm length and thermal history on crystallinity was investigated by differential scanning calorimetry (DSC) and wide-angle x-ray scattering (WAXS). It was shown that annealing increased the melting temperature (T ◦ ◦ m ) and crystallinity. However, annealing at 140 ◦ C for 14 d also caused significant solid-state transesterification. In addition, crystallites composed of s-PLAs with extended arms and, simultaneously, crystallites composed exclusively of extended rings were formed, identified by their typical "sawtooth" pattern in the MALDI mass spectra. Small angle x-ray scattering (SAXS) indicated that the crystal thickness was lower than that of linear PLAs annealed under identical conditions, but increased upon annealing at 140 C.
KW - MALDI-TOF MS
KW - Polylactide
KW - Crystallisation
KW - AStar-shaped polymers
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-636832
DO - https://doi.org/10.1016/j.polymer.2025.128709
SN - 0032-3861
VL - 334
SP - 1
EP - 11
PB - Elsevier Ltd.
AN - OPUS4-63683
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Kricheldorf, Hans R.
A1 - Weidner, Steffen
T1 - H2O-Initiated Polymerization of L-Lactide
N2 - Water-initiated ring-opening polymerizations (ROPs) of L-lactide (LA) were performed in bulk at 140 °C, whereupon 11 different salts or complexes of low-toxic metal ions such as tin (II), Zn(II), Zr(IV), and Bi(III) were used as catalysts. Only four catalysts gave satisfactory results despite a long reaction time (24 h). The influence of the temperature was studied with tin (II) 2-ethylhexanoate (SnOct2), dibutyltin oxide (Bu2SnO), and zinc bis-acetylacetonate (Zn(acac)2) and zirconium acetylacetonate (Zr(acac)4). With SnOct2, Bu2SnO and Zr(acac)4 the time was varied at 140 °C to compare their reactivity. Furthermore, two series of ROPs were carried out with variation of the LA/H2O ratio to verify the control of the molecular weight by the monomer-initiator ratio. Bi- or tri-modal molecular weight distributions (MWD) were found for most of the ROPs and bimodal melting endotherms in the differential scanning calorimetry (DSC) heating traces. The thickness and dependence of the 3D packing of the crystallites were monitored by small-angle X-ray scattering (SAXS) measurements.
KW - MALDI-TOF MS
KW - Polylactide
KW - Ring-opening polymerization
KW - Crystallization
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-628761
DO - https://doi.org/10.1007/s10924-025-03565-w
SN - 1572-8919
VL - 33
IS - 6
SP - 2843
EP - 2857
PB - Springer Science and Business Media LLC
CY - New York, NY
AN - OPUS4-62876
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Kricheldorf, Hans R.
A1 - Weidner, Steffen
A1 - Scheliga, Felix
T1 - Polycondensation of L-lactic acid: a deeper look into solid state polycondensation
N2 - L-Lactic acid (LA) was condensed in the presence of SnCl2 or 4-toluenesulfonic acid (TSA) at 140 °C, and chain growth without cyclization was observed. In addition, poly(L-lactic acid)s (PLAs) with a degree of polymerization (DP) of 25, 50 or 100 were prepared by water-initiated ring-opening polymerization (ROP). These PLAs were annealed in the solid state at 140 °C and 160 °C in the presence of tin(II) 2-ethylhexanoate (SnOct2, SnCl2 or TSA). The changes in the molar mass distribution and in the topology were characterized by means of matrix-assisted laser desorption/ionization time-of-flight (MALDI-TOF) mass spectrometry and size exclusion chromatography (SEC). With increasing time, fewer side reactions caused higher molar masses and increasing fractions of cyclic polylactides (cPLA) were obtained. Their “saw tooth” pattern in the MALDI-TOF mass spectra indicated the formation of extended ring crystallites in the solid state. TSA was the most active catalyst and caused fewer side reactions than SnCl2, which was the least reactive catalyst. Acetylation of the CH-OH end groups hindered polycondensation and prevented the formation of cPLAs. Reaction mechanisms will be discussed.
KW - MALDI-TOF MS
KW - Polycondensation
KW - Polylaktide
KW - Solid state
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-625271
DO - https://doi.org/10.1039/d4py01191k
SN - 1759-9962
SP - 1
EP - 9
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-62527
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Rösler, Alexander
A1 - Weidner, Steffen
A1 - Klamroth, Tillmann
A1 - Müller, Axel HE
A1 - Schlaad, Helmut
T1 - Kinetics of anionic polymerization of β‐myrcene in hydrocarbon solvents
N2 - AbstractThe kinetics of anionic polymerization of β‐myrcene initiated by sec‐butyllithium were examined in saturated and unsaturated hydrocarbon solvents, i.e. cyclohexane, cyclohexene, 4‐vinylcyclohexene and dl‐limonene. Polymerizations usually proceeded in a living manner, i.e. in the absence of termination and chain transfer reactions, in all solvents, to produce well‐defined polymyrcenes with high content (85%) of cis‐1,4 units. However, polymyrcenyllithium chains exhibited limited long‐term stability in 4‐vinylcyclohexene solution, most probably due to chain transfer to solvent. Reaction orders with respect to the concentration of active chains were found to be one‐quarter in cyclohexane increasing to one‐half in unsaturated solvents, indicating that the polymyrcenyllithium chains are present as tetrameric or dimeric associates, respectively. Apparent activation energies were found to be 81 kJ mol−1 in cyclohexane and 77 kJ mol−1 in dl‐limonene solution, which are close to the values obtained by quantum chemical calculations. © 2025 The Author(s). Polymer International published by John Wiley & Sons Ltd on behalf of Society of Chemical Industry.
KW - Myrcene
KW - Anionic polymerization
KW - Reaction order
KW - Activation energy
KW - Microstructure
KW - Quantum chemical calculation
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-636840
DO - https://doi.org/10.1002/pi.6772
SN - 0959-8103
SP - 1
EP - 8
PB - Wiley
AN - OPUS4-63684
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Kricheldorf, H. R.
A1 - Weidner, Steffen
T1 - Syntheses of cyclic polylactides and the problem of catenane formation
N2 - Cyclic poly(L-lactide)s (PLAs) were prepared in bulk either by ring-expansion polymerization (REP) or by ring-opening polymerization (ROP) with simultaneous polycondensation (ROPPOC). In contrast to REP the latter method involves formation of linear chains and thus, may involve formation of polydisperse catenanes that affect crystallization. The reprecipitated PLAs were annealed at 120 °C and compared with regard to melting temperature (Tm) and melting enthalpy (ΔHm). For similar molar masses the PLAs prepared by REP and ROPPOC had almost identical Tm's and crystallinities. Furthermore, the influence of REP and ROPPOC catalysts on the morphology of the virgin reaction products was compared.
KW - MALDI-TOF MS
KW - Catenane
KW - Polylactide
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-625061
DO - https://doi.org/10.1039/d4ra08683j
VL - 15
IS - 5
SP - 3686
EP - 3692
PB - RSC
AN - OPUS4-62506
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Rösler, Alexander
A1 - Weidner, Steffen
A1 - Klamroth, Tillmann
A1 - Müller, Axel H. E.
A1 - Schlaad, Helmut
T1 - Kinetics of anionic polymerization of β‐myrcene in hydrocarbon solvents
N2 - The kinetics of anionic polymerization of β‐myrcene initiated by sec‐butyllithium were examined in saturated and unsaturated hydrocarbon solvents, i.e. cyclohexane, cyclohexene, 4‐vinylcyclohexene and dl‐limonene. Polymerizations usually proceeded in a living manner, i.e. in the absence of termination and chain transfer reactions, in all solvents, to produce well‐defined polymyrcenes with high content (85%) of cis‐1,4 units. However, polymyrcenyllithium chains exhibited limited long‐term stability in 4‐vinylcyclohexene solution, most probably due to chain transfer to solvent. Reaction orders with respect to the concentration of active chains were found to be one‐quarter in cyclohexane increasing to one‐half in unsaturated solvents, indicating that the polymyrcenyllithium chains are present as tetrameric or dimeric associates, respectively. Apparent activation energies were found to be 81 kJ mol−1 in cyclohexane and 77 kJ mol−1 in dl‐limonene solution, which are close to the values obtained by quantum chemical calculations.
KW - MALDI-TOF MS
KW - Anionic polymerization
KW - β‐myrcene
KW - Kinetics
KW - Reaction order
KW - Activation energy
KW - Microstructure
KW - Quantum chemical calculations
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-630900
DO - https://doi.org/10.1002/pi.6772
SN - 1097-0126
SP - 1
EP - 8
PB - Wiley
CY - New York, NY
AN - OPUS4-63090
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Kricheldorf, Hans R.
A1 - Weidner, Steffen
T1 - Zwitterionic polymerization of glycolide catalyzed by pyridine
N2 - The usefulness of various N- and P-based catalysts for syntheses of cyclic polyglycolide via zwitterionic polymerization of glycolide was examined. Most catalysts produced discolored, largely insoluble polyglycolides consisting of cycles and unidentified byproducts. Soluble, cyclic polyglycolides were obtained using neat pyridine as catalyst at 120 °C, 100 °C, 80 °C, and even at 60 °C. The number-average molecular weights were extremely low and depended slightly on the glycolide-to-pyridine ratio. Three different mass distributions of the cycles were detected by mass spectrometry, depending on the reaction conditions. The cyclic polyglycolides were also characterized by differential scanning calorimetry (DSC) and small-angle X-ray scattering (SAXS) measurements. The SAXS data in combination with the mass spectra indicate that the majority of the cycles form extended-ring crystallites
KW - MALDI-TOF MS
KW - Polylactide
KW - Polymerization
KW - Zitterions
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-639748
DO - https://doi.org/10.1039/d5py00762c
SN - 1759-9954
SP - 1
EP - 9
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-63974
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Rösler, Alexander
A1 - Weidner, Steffen
A1 - Klamroth, Tillmann
A1 - Müller, Axel HE
A1 - Schlaad, Helmut
T1 - Kinetics of anionic polymerization of β‐myrcene in hydrocarbon solvents
N2 - AbstractThe kinetics of anionic polymerization of β‐myrcene initiated by sec‐butyllithium were examined in saturated and unsaturated hydrocarbon solvents, i.e. cyclohexane, cyclohexene, 4‐vinylcyclohexene and dl‐limonene. Polymerizations usually proceeded in a living manner, i.e. in the absence of termination and chain transfer reactions, in all solvents, to produce well‐defined polymyrcenes with high content (85%) of cis‐1,4 units. However, polymyrcenyllithium chains exhibited limited long‐term stability in 4‐vinylcyclohexene solution, most probably due to chain transfer to solvent. Reaction orders with respect to the concentration of active chains were found to be one‐quarter in cyclohexane increasing to one‐half in unsaturated solvents, indicating that the polymyrcenyllithium chains are present as tetrameric or dimeric associates, respectively. Apparent activation energies were found to be 81 kJ mol−1 in cyclohexane and 77 kJ mol−1 in dl‐limonene solution, which are close to the values obtained by quantum chemical calculations. © 2025 The Author(s). Polymer International published by John Wiley & Sons Ltd on behalf of Society of Chemical Industry.
KW - Myrcene
KW - Anionic polymerization
KW - MALDI TOF MS
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-649039
DO - https://doi.org/10.1002/pi.6772
SN - 0959-8103
SP - 1
EP - 8
PB - Wiley
AN - OPUS4-64903
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Kricheldorf, Hans R.
A1 - Weidner, Steffen
T1 - Polymerization of L‐Lactide Catalyzed by Metal Acetylacetonate Complexes
N2 - ABSTRACTRing‐opening polymerizations (ROPs) of l‐lactide (LA) were performed at 120°C, 140°C, 150°C, and 180°C in bulk catalyzed by acetylacetonate (acac) complexes of manganese(II), nickel(II), copper(II), zirconium(IV), dibutyltin(IV), and vanadyl(V). These experiments revealed that only the acac complexes of Zr and Bu2Sn were reactive enough to enable quantitative polymerization within a few hours. Further ROPs with Bu2Sn(acac)2 and Zr(acac)4 showed that Bu2Sn(acac)2 had a slightly lower reactivity than the Zr complex. The ROPs catalyzed with Zr(acac)4 yielded number average molecular weights (Mn) up to 70,000 g mol−1. The matrix‐assisted laser desorption/ionization time‐of‐flight (MALDI‐TOF) mass spectra indicated an exclusive formation of cycles in the mass range of up to m/z 13,000 for Zr(acac)4 and up to m/z 18,000 for Bu2Sn(acac)2. Unusually high melting temperatures (187°C–192°C) were also achieved along with high crystallinities. Furthermore, four lactide/glycolide copolymerizations catalyzed by Zr(acac)4 were performed, and the topology and the extent of transesterification were characterized by MALDI‐TOF mass spectrometry and 13C NMR spectroscopy.
KW - MALDI-TOF MS
KW - Polycondensation
KW - Acetylacetonate
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-639754
DO - https://doi.org/10.1002/pol.20250788
SN - 2642-4150
SP - 1
EP - 9
PB - Wiley Periodicals LLC.
AN - OPUS4-63975
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Falkenhagen, Jana
A1 - Dalgic, Mete-Sungur
A1 - Weidner, Steffen
T1 - Quantitative MALDI-TOF Mass Spectrometry of Star-Shaped Polylactides Based on Chromatographic Hyphenation
N2 - The end groups of three- and four-arm star-shaped polylactides (PLA) with trimethylolpropane and pentaerythritol core structures were functionalized with acetic acid. Reaction products with different degrees of functionalization were analyzed by matrix-assisted laser desorption/ionization time-of-flight (MALDI-TOF) mass spectrometry. Additional gradient elution liquid adsorption chromatography (GELAC) measurements were performed to determine the degree of functionalization. This technique enabled clear separation and sufficient quantification of the formed species. These chromatographic data could be used inversely to quantify mass spectrometric results, which are usually biased by the unknown ionization probabilities of different polymer end group structures. Our results showed that, in this particular case, the peak intensity in the MALDITOF mass spectra can be used to semiquantitatively determine the degree of functionalization in incompletely functionalized multiarm PLA.
KW - Polylactides
KW - MALDI-TOF-MS
KW - Gradient elution liquid adsorption chromatography
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-625292
DO - https://doi.org/10.1021/jasms.4c00491
SN - 1879-1123
SP - 1
EP - 9
PB - American Chemical Society (ACS)
AN - OPUS4-62529
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Recknagel, Sebastian
A1 - Richter, Silke
A1 - Hoppe, Marion
A1 - Meckelburg, Angela
A1 - Prinz, Carsten
A1 - Roik, Janina
A1 - Abad Andrade, Carlos Enrique
T1 - Powering precision: development of a certified reference material for elemental composition analysis of lithium nickel manganese cobalt oxide (Li-NMC) cathode material for lithium-ion batteries
N2 - This work presents the development and certification of the world’s first certified reference material (CRM), BAM-S014, for a lithium nickel manganese cobalt oxide (LiNi0.33Mn0.33Co0.33O2 or Li-NMC 111) cathode material—an integral component in high-energy-density lithium-ion batteries that power electric vehicles (EVs), portable electronics, and stationary energy storage systems. By providing certified mass fractions for 11 elements, this CRM addresses a critical need for accurate and traceable elemental analysis, supporting quality control and regulatory compliance in the global battery industry. Ensuring reliable and harmonized measurements supports the efficient use of resources, including the reuse of recycled materials, and ultimately helps maintain product performance and safety. The values were assigned through an interlaboratory comparison involving 16 participating laboratories and various analytical techniques such as inductively coupled plasma optical emission spectrometry (ICP-OES), inductively coupled plasma mass spectrometry (ICP-MS), X-ray fluorescence (XRF) spectrometry, and combustion analysis. In addition to chemical characterization, the certification process includes homogeneity and stability testing of the candidate material. Details are provided on the analytical methods used for chemical characterization and the calculation of the uncertainties of the certified mass fractions. In addition to detailing the development of the CRMs, this work provides an overview of ongoing standardization activities in Li-component analysis, thereby guiding the calibration of analytical methods and contributing to the establishment of globally accepted standards for evaluating energy storage materials and advancing sustainable mobility and clean energy solutions.
KW - Certified reference material
KW - Lithium nickel manganese cobalt oxide
KW - LNMC
KW - Lithium-ion battery
KW - Cathode material
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-643763
DO - https://doi.org/10.1007/s00216-025-05766-7
SN - 1618-2642
VL - 417
IS - 12
SP - 2643
EP - 2653
PB - Springer Nature
AN - OPUS4-64376
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Kossatz, Philipp
A1 - Mezhov, Alexander
A1 - Andresen, Elina
A1 - Prinz, Carsten
A1 - Schmidt, Wolfram
A1 - Resch-Genger, Ute
T1 - Assessing the Applicability of Lanthanide-Based Upconverting Nanoparticles for Optically Monitoring Cement Hydration and Tagging Building Materials
N2 - Chemically stable, lanthanide-based photon upconversion micro- and nanoparticles (UCNPs) with their characteristic multicolor emission bands in the ultraviolet (UV), visible (vis), near-infrared (NIR), and short-wave infrared (SWIR) arepromising optical reporters and barcoding tags. To assess the applicability of UCNPs for the monitoring of early stage cement hydration processes and as authentication tags for cementitious materials, we screened the evolution of the luminescence of Selfmade core-only NaYF4:Yb,Er UCNPs and commercial μm-sized Y2O2S:Yb,Er particles during the first stages of cement hydration, which largely determines the future properties of the hardened material. Parameters explored from the UCNP side included particle size, morphology, surface chemistry or coating, luminescence properties, and concentration in different cement mixtures. From the cement side, the influence of the mineral composition of the cement matrix was representatively examined for ordinary Portland cement (OPC) and its constituents tricalcium aluminate (C3A), tricalcium silicate (C3S), and gypsum at different water to cement ratios. Based on reflection and luminescence measurements, enabling online monitoring, which were complemented by XRD and isothermal heat-flow calorimetric measurements to determine whether the incorporation of these particles could impair cement hydration processes, well suited lanthanide particle reporters could be identified as well as application conditions. In addition, thereby the reporter influence on cement hydration kinetics could be minimized while still preserving a high level of information content. The best performance for the luminescence probing of changes during early stage cement hydration processes was observed for 25 nm-sized oleate (OA)-coated UCNPs added in a concentration of 0.1 wt %. Higher UCNP amounts of 1.0 wt % delayed cement hydration processes size- and surface coatingspecifically in the first 24 h. Subsequent luminescence stability screening studies performed over a period of about one year support the applicability of UCNPs as optical authentication tags for construction materials.
KW - Quality assurance
KW - Fluorescence
KW - Nano
KW - Particle
KW - Synthesis
KW - Quantum yield
KW - NIR
KW - Mechanism
KW - Characterization
KW - XRD
KW - Calorimetry
KW - Advanced material
KW - Cement
KW - Monitoring
KW - Surface
KW - Size
KW - Lifetime
KW - Barcode
KW - Lanthanide
KW - Upconversion
KW - Encoding
KW - Method
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-638318
DO - https://doi.org/10.1021/acsomega.5c02236
SN - 2470-1343
VL - 10
IS - 29
SP - 31587
EP - 31599
PB - ACS Publications
CY - Washington, DC
AN - OPUS4-63831
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - CONF
A1 - Radtke, Martin
T1 - ChatGPT and epics: LLM enhanced control systems for synchrotron Beamlines
N2 - The presentation describes how large language models (LLMs) such as ChatGPT can be integrated with the EPICS control system to improve the automation and usability of synchrotron beamlines like the BAMline at BESSY II.
It explains how LLMs can interpret natural language instructions, translate them into EPICS commands, and interact with experimental tools to perform complex tasks such as moving motors, running scans, or adjusting beamline components. The system, named P.E.T.E.R. (Performance Enhancing Technology for Experimental Research), supports features like multi-step reasoning, Python scripting, feedback loops, multilingual input, and voice control using OpenAI’s ChatGPT and Whisper.
T2 - Workshop "BAM - Fraunhofer Materials LLM days"
CY - Tübingen, Germany
DA - 03.07.2025
KW - Chatgpt
KW - LLM
KW - EPICS
KW - BAMline
KW - Sanchrotron
PY - 2025
AN - OPUS4-64478
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - CONF
A1 - de Oliveira Guilherme Buzanich, Ana
T1 - Bridging Structure and Electronic State: Real-time XES–XRD Fusion for Functional Alloys
N2 - We present a unified X-ray Emission Spectroscopy (XES) and X-ray Diffraction (XRD) approach for real-time, in situ characterization of materials, demonstrated on Co₂FeSi Heusler alloys under varied heat treatments. The combination of XES and XRD is particularly well-suited to Heusler alloys, where subtle changes in atomic ordering and electronic structure (e.g. site occupancy, hybridization, and spin state) are tightly interdependent and critical for their magnetic and transport properties. In addition, this method enables more efficient materials design by reducing experimental iterations through comprehensive structural and electronic analysis. Developed at the mySpot beamline at BESSY-II, the platform integrates (a) digital twin-based experiment planning, (b) open-source XES spectral simulations, (c) an optimized single-shot, two-element XES setup with sub-pixel resolution for enhanced energy precision, and (d) result-driven beamtime utilization. With an unprecedented synchronized XES-XRD platform, we aim to shed light on how diffusion-controlled processes in Heusler alloys and double perovskites at elevated temperatures establish the formation of specific phases with distinct structure types in real time. This, in turn, strongly impacts the functional properties of the materials under scrutiny.
T2 - XLIV Colloquium Spectroscopicum Internationale
CY - Ulm, Germany
DA - 27.07.2025
KW - Multimodal
KW - X-ray spectroscopy
KW - X-ray diffraction
KW - Functional alloys
PY - 2025
AN - OPUS4-63991
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - CONF
A1 - Radtke, Martin
T1 - Illuminating the Past, Shaping the Future: Advanced Technologies in Gold Analysis and Beamline Control
N2 - The presentation explores how synchrotron radiation is used for non-destructive and highly precise analysis of gold artifacts.
It explains how synchrotron radiation provides extremely bright and tunable X-rays that can examine very small areas with great accuracy. These features make it ideal for studying cultural heritage objects without damaging them. The presentation highlights case studies such as the Nebra Sky Disk, the Hiddensee gold jewelry, Phoenician ivory, and Egyptian gold from Abydos. These examples show how synchrotron-based techniques reveal details about the origin, composition, and manufacturing of ancient gold.
A major focus is the Bernstorf gold discovery in Bavaria. Over several years, different analytical methods, including synchrotron X-ray fluorescence, were applied to test whether the gold was genuinely ancient. The studies found nearly pure gold, sparking debate about whether such purity could be achieved in the Bronze Age.
In the final part, the presentation connects this research with modern developments in automation and artificial intelligence. It describes how beamline experiments can be controlled through the EPICS system, Python scripting, and AI tools such as ChatGPT and Whisper, enabling intelligent and voice-assisted operation.
T2 - Seminar Strahlenphysikalische Anwendungen in Technik und Medizin
CY - Wien, Austria
DA - 29.01.2025
KW - Synchrotron
KW - BAMline
KW - AI
KW - Gold
KW - XRF
PY - 2025
AN - OPUS4-64477
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - CONF
A1 - Cakir, Cafer Tufan
A1 - de Oliveira Guilherme Buzanich, Ana
A1 - Radtke, Martin
T1 - A Digital Twin Workflow for Optimizing X-ray Emission Spectroscopy (XES) Parameters in Material Science
N2 - In this contribution, I present a digital twin-based workflow designed to optimize experimental parameters in X-ray emission spectroscopy (XES), with a focus on reproducibility, data integration, and alignment with FAIR (Findable, Accessible, Interoperable, Reusable) principles in materials science and engineering (MSE). The developed pipeline begins with automated retrieval of crystallographic information from the Materials Project database based on a given sample composition. This structural data is then used to simulate the corresponding XES spectra using FDMNES, allowing for accurate prediction of element-specific emission lines.
The simulated emission lines are fed into an X-ray tracing (XRT) module, which builds a virtual replica of the experimental setup. This digital twin environment enables predictive modeling of spectrometer performance based on geometric configurations. The optimization focuses on two key parameters: the choice of the analyzing crystal and the distance between the sample and crystal (which also defines the crystal–detector distance due to Bragg condition constraints). An active learning algorithm is employed to iteratively adjust these parameters in order to achieve a desired energy-per-pixel (E/pixel) resolution with minimal intensity loss, enabling efficient, data-driven experimental planning.
By integrating data-driven simulations with real-time optimization strategies, this workflow supports efficient experiment planning while minimizing resource consumption and human error. Furthermore, all stages of the process—from data collection and simulation to optimization and visualization—are structured to ensure traceability and interoperability, facilitating future reuse and collaborative research.
I hope this contribution aligns well with the topic “Workflows for FAIR MSE Data” and offers a concrete example of how digital twins can be harnessed to improve the design, execution, and documentation of spectroscopy experiments in the MSE domain.
T2 - Opportunities and Challenges of FAIR Data at Photon and Neutron Facilities
CY - Bad Honnef, Germany
DA - 12.10.2025
KW - Digital-Twin
KW - XES
KW - Optimization
KW - Machine Learning
PY - 2025
AN - OPUS4-64676
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - CONF
A1 - Cakir, Cafer Tufan
A1 - de Oliveira Guilherme Buzanich, Ana
A1 - Radtke, Martin
T1 - Digital Twin for Multimodal Synchrotron Experiments
N2 - In this contribution, I present a digital twin-based workflow designed to optimize experimental parameters in X-ray emission spectroscopy (XES), with a focus on reproducibility, data integration, and alignment with FAIR (Findable, Accessible, Interoperable, Reusable) principles in materials science and engineering (MSE). The developed pipeline begins with automated retrieval of crystallographic information from the Materials Project database based on a given sample composition. This structural data is then used to simulate the corresponding XES spectra using FDMNES, allowing for accurate prediction of element-specific emission lines.
The simulated emission lines are fed into an X-ray tracing (XRT) module, which builds a virtual replica of the experimental setup. This digital twin environment enables predictive modeling of spectrometer performance based on geometric configurations. The optimization focuses on two key parameters: the choice of the analyzing crystal and the distance between the sample and crystal (which also defines the crystal–detector distance due to Bragg condition constraints). An active learning algorithm is employed to iteratively adjust these parameters in order to achieve a desired energy-per-pixel (E/pixel) resolution with minimal intensity loss, enabling efficient, data-driven experimental planning.
By integrating data-driven simulations with real-time optimization strategies, this workflow supports efficient experiment planning while minimizing resource consumption and human error. Furthermore, all stages of the process—from data collection and simulation to optimization and visualization—are structured to ensure traceability and interoperability, facilitating future reuse and collaborative research.
I hope this contribution aligns well with the topic “Workflows for FAIR MSE Data” and offers a concrete example of how digital twins can be harnessed to improve the design, execution, and documentation of spectroscopy experiments in the MSE domain.
T2 - MSE Research Data Forum 2025
CY - Siegburg, Germany
DA - 08.07.2025
KW - Multi Modal
KW - XRD
KW - XRF
KW - Optimization
PY - 2025
AN - OPUS4-63794
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - THES
A1 - Cakir, Cafer Tufan
T1 - Optimization of depth resolved X-ray absorption spectroscopy in grazing emission mode for characterizing compositionally complex alloys
N2 - Layered materials are fundamental to technological advancements, offering distinct properties that differentiate them from bulk materials. In electronics, for instance, thin-film transistors (TFTs) are used to enhance charge transport and flexibility, thereby improving device performance. In the same way, thin-film photovoltaic devices used in renewable energy use strategic layering to absorb light more efficiently and separate electron-hole pairs more effectively, which leads to higher energy conversion efficiency. In recent decades, the development of new alloys has highlighted the importance of layered materials in another context. Compositionally complex alloys, for example, form multiple oxide layers on their surfaces when they oxidize. Studying these corrosion layers is crucial for understanding material-environment interactions.
Typical surface analysis techniques, including X-ray photoelectron spectroscopy (XPS), secondary ion mass spectrometry (SIMS), and Meitner-Auger electron spectroscopy (MAES), provide valuable insights but are constrained by their requirements for high Vacuum conditions and their limited depth analysis. In contrast, X-ray absorption near-edge structure (XANES) spectroscopy presents a versatile and advantageous alternative. It operates effectively under ambient conditions and allows time-resolved measurements, enhancing the analysis of materials in real-time as they undergo structural and compositional changes. This adaptability broadens the scope for material analysis, allowing for a more comprehensive understanding of dynamic processes.
Grazing Emission X-ray Fluorescence (GEXRF) spectroscopy stands out as a nondestructive, depth-resolved, element-specific characterization technique important for collecting depth-resolved information at the nanometer scale. Its ability to collect in-Depth resolved information based on the grazing emission angle of the fluorescence Radiation makes it ideal for investigating thin films, corrosion layers, and interfaces within layered materials. The integration of XANES in emission mode with GEXRF enables detailed exploration of the chemical states of the analyzed atom and provides depth-resolved information. This study discusses grazing emission X-ray absorption near-edge structure spectroscopy (GEXANES), a novel layer analysis technique that is created by integrating these two methods.
This study also innovatively combines machine learning with GEXANES spectroscopy to reduce experimental times. By using active learning, a subset of machine learning, it refines the data acquisition process, enabling more efficient and streamlined methods. The application of active learning in this context illustrates the potential of data-driven approaches to transform experimental methodologies, particularly in resource-limited environments such as synchrotron facilities, thereby accelerating scientific research and discovery.
KW - Angle resolved XRF
KW - GEXRF
KW - BO
KW - Active Learning
KW - XRF
PY - 2025
DO - https://doi.org/10.34726/hss.2025.101302
SP - 1
EP - 129
CY - Technische Univeristät Wien
AN - OPUS4-63793
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - INPR
A1 - Battistella, Beatrice
A1 - Revill, Adam
A1 - Venzago, Cornel
A1 - Hoffmann, Volker
A1 - Agudo Jacome, Leonardo
A1 - Al-Sabbagh, Dominik
A1 - Recknagel, Sebastian
A1 - Abad Andrade, Carlos Enrique
T1 - Depth-Resolved Lithium Isotope Fractionation as a Diagnostic of Interphase Evolution and Degradation in Lithium Ion Batteries
N2 - Lithium isotopic fractionation is well-established in dynamic geochemical systems; however, its role in lithium-ion batteries (LIBs) remains uninvestigated. Herein, we report the first depth-resolved demonstration that isotopic separation occurs during Li-ion cell operation whose magnitude depends on the cycling history. Using depth-resolved glow discharge mass spectrometry, we monitored the 7Li/6Li ratio in LiNi0.333Mn0.333Co0.333O2 (NMC111)||graphite coin cell electrodes at defined life-cycle stages. Different charging rates were examined to get mechanistic insight into kinetic and thermodynamic control in the fractionation process. Although pristine electrodes exhibit a uniform isotopic ratio, cycled electrodes show a distinct 7Li enrichment in the positive electrode and a corresponding accumulation of 6Li at the surface of the negative electrode. The degree of isotopic separation varies with the charging rate. Isotopic signatures correlate with capacity fading, indicating lithium isotope mapping as a sensitive diagnostic tool for tracking electrode degradation and the evolution of the electrode–electrolyte interphases in LIBs.
KW - Li-ion batteries
KW - Lithium isotopes
KW - Post-mortem analysis
KW - GD-MS
KW - Depth profile
KW - Mass spectrometry
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-651287
DO - https://doi.org/10.26434/chemrxiv-2025-5rvlk
SP - 1
EP - 19
AN - OPUS4-65128
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - CONF
A1 - Abad Andrade, Carlos Enrique
T1 - Tracking Lithium-Ion Battery Ageing via Lithium Isotope Fractionation
N2 - Lithium-ion batteries power portable devices, electric vehicles, and stationary power grids, yet hidden aging reactions still shorten their service life and raise concerns about cost and safety. An analytical proxy is needed to report these reactions and accelerate product development, quality control, and recycling. Here, we demonstrate that subtle shifts in the natural 7Li/6Li ratio accurately record the two decisive stages of cell aging, solid-electrolyte interphase (SEI) formation and field-driven aging, which can be detected using multi-collector ICP-MS.
Because Li is easily stripped from digested electrodes or electrolyte in a one-step cation-exchange column, high-purity solutions reach the spectrometer in minutes. A streamlined MC-ICP-MS run yields a δ7LiLSVEC precision of 0.4 ‰, enabling dozens of battery fractions to be analyzed per day.
Applying the workflow to LiCoO2 coin cells as models, sampled from pristine to 700 cycles, reveals a clear isotopic narrative. During the first ≈45 cycles, 7Li leaves the LiCoO2 lattice, dissolves into the electrolyte, and is locked in the SEI on graphite, driving cathode δ7Li from +8 to –10 ‰ and raising the anode to +13 ‰ while capacity drops by 10 %. After the interphase matures, the electric field takes over: the lighter 6Li migrates faster to the anode, 7Li accumulates in the contracting Li1-xCoO2 lattice, and the bulk separation factor rises to α≈1.045 by 700 cycles. The δ7Li curve flattens roughly 70 cycles before capacity falls to 80%, providing an early warning of end-of-life. Isotopic gradients scale linearly with impedance growth, SEI thickness, and crack density confirmed by LA-ICP-MS mapping, FIB-SEM, XANES, and EXAFS.
Although each data point requires one cell, lithium-isotope fractionation provides direct, element-specific, and structural fatigue insight unavailable from non-destructive tests. The straightforward chemistry and fast MC-ICP-MS routine make the approach practical for targeted aging studies, additive screening, and forensic autopsies, complementing high-throughput electrochemical methods and supporting the design of longer-lived batteries.
T2 - SciX 2025
CY - Covington, KY, USA
DA - 05.10.2025
KW - Isotope
KW - Lithium
KW - MC-ICP-MS
KW - MICAP-MS
KW - Isotope fractionation
KW - Battery
PY - 2025
AN - OPUS4-64879
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Fink, Friedrich
A1 - Stawski, Tomasz M.
A1 - Emmerling, Franziska
A1 - Falkenhagen, Jana
T1 - A novel machine-learning approach to unlock technical lignin classification by NIR spectroscopy - bench to handheld
N2 - In this research, the utilization of near-infrared (NIR) spectroscopy in conjunction with advanced machine learning methods is investigated for categorizing technical lignins obtained from different biomass sources and industrial procedures. Technical lignins, such as kraft, organosolv and lignosulfonates, have different chemical compositions, which continue to make uniform characterization and application in sustainable sectors extremely difficult. Fast, universally accessible analytics combined with data analysis is still an open question. For the first time three distinct NIR spectrometers—a high-performance benchtop system, a mid-priced compact device, and an economical handheld unit—were utilized to record NIR spectra of 31 unique lignin samples. The spectra underwent pre-processing through standard normal variate (SNV) transformation and Savitzky-Golay derivatives to amplify spectral features and decrease noise. Principal component analysis (PCA) was employed to reduce data complexity and extract crucial characteristics for classification purposes. Subsequently, four machine learning algorithms—Support Vector Machines (SVM), Gaussian Naive Bayes (GNB), Gaussian Process Classification (GPC), and Decision Tree Classification (DTC)—were implemented for the classification of the lignin samples. The DTC model exhibited the highest accuracy among them across different spectrometers. Although the benchtop spectrometer produced the most precise outcomes, the compact NeoSpectra system also displayed potential as a cost-efficient option. Nonetheless, the restricted spectral coverage of the handheld NIRONE spectrometer resulted in reduced classification accuracy. Our discoveries highlight the capability of NIR spectroscopy, combined with robust data analysis techniques, for the swift and non-destructive classification of technical lignins, facilitating their improved utilization in sustainable fields.
KW - Technical lignins
KW - NIR spectroscopy
KW - Classification
KW - Machine-learning
KW - PCA
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-634518
DO - https://doi.org/10.1016/j.chemolab.2025.105467
SN - 0169-7439
VL - 264
SP - 1
EP - 10
PB - Elsevier B.V.
CY - Amsterdam
AN - OPUS4-63451
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - INPR
A1 - Morcillo, Dalia
A1 - Oelze, Marcus
A1 - Seena Prem, Pranav
A1 - de Oliveira Guilherme Buzanich, Ana
A1 - Emmerling, Franziska
A1 - Recknagel, Sebastian
A1 - Panne, Ulrich
A1 - Abad Andrade, Carlos Enrique
T1 - Lithium isotope fractionation as an early indicator of degradation mechanisms in lithium-ion batteries
N2 - Aging in lithium-ion batteries (LIBs) degrades performance and hinders sustainability, demanding advanced diagnostics for early failure prediction. We investigate lithium isotope fractionation (LIF) as an innovative probe of degradation in lithium cobalt oxide (LCO) coin cells aged over 0−700 cycles. High-precision multi-collector inductively coupled plasma mass spectrometry (MC-ICP-MS) quantified δ7Li variations across cell stages: non-cycled (0 cycles), newly formed (5 cycles), semi-aged (250 cycles), and fully aged (700 cycles). During early cycling (≤ 45 cycles), chemical processes drive 7Li enrichment at the anode (δ7Li vs LSVEC = +12 ‰) through solid electrolyte interphase (SEI) formation, while the cathode depletes in 7Li (δ7Li vs LSVEC = −0.7 ‰). Beyond 45 cycles, electric field-induced migration predominates, promoting 6Li intercalation into the anode and increasing the δ7Li of the cathode by 8.1 ‰. Mass balance verifies isotope conservation, attributing shifts to redistribution and trapping. Complementary electrochemical impedance spectroscopy (EIS) and X-ray absorption spectroscopy and diffraction confirm SEI expansion, cobalt oxidation, lattice shrinkage, and changes in electrode structure, corroborating LIF trends. Notably, a δ7Li inflection at approximately 270 cycles anticipates end-of-life by 70 cycles, surpassing traditional methods in sensitivity. LIF emerges as a predictive indicator of aging mechanisms, informing optimized designs for durable LIBs.
KW - Lithium isotope fractionation
KW - Lithium-ion batteries
KW - Degradation mechanisms
KW - LiCoO2 cathodes
KW - LCO
KW - Isotopic tracing
KW - Lithium isotopes
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-650945
DO - https://doi.org/10.26434/chemrxiv-2025-16lvq
SP - 1
EP - 19
AN - OPUS4-65094
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Hoque, Maroof Arshadul
A1 - Sommerfeld, Thomas
A1 - Lisec, Jan
A1 - Das, Prasenjit
A1 - Prinz, Carsten
A1 - Heinekamp, Christian
A1 - Stolar, Tomislav
A1 - Etter, Martin
A1 - Rosenberger, David
A1 - George, Janine
A1 - Bhattacharya, Biswajit
A1 - Emmerling, Franziska
T1 - Mechanochemically Synthesized Covalent Organic Framework Effectively Captures PFAS Contaminants
N2 - Per‐ and polyfluoroalkyl substances (PFAS) are persistent environmental contaminants that pose significant health risks, prompting urgent efforts to develop effective removal methods and adsorbers. Covalent organic frameworks (COFs) are metal‐free adsorbers with high stability and tunable porosity. A highly crystalline COF is synthesised mechanochemically using 1,3,5‐tris(4‐aminophenyl)benzene (TAPB) and 1,3,5‐triformylbenzene (TFB). The formation dynamics are monitored in real time with time‐resolved in situ synchrotron X‐ray diffraction. The TAPB‐TFB COF demonstrates good efficiency in eliminating PFAS from water. Perfluorooctanoic acid (PFOA) and perfluorooctanesulfonic acid (PFOS) are effectively extracted, and most of the adsorption occurred within the first 10 min. Additionally, X‐ray photoelectron spectroscopy, Fourier transform infrared spectroscopy, and DFT calculations are employed to elucidate the molecular interactions between PFAS and the COF framework. The rapid and efficient removal of PFAS makes TAPB‐TFB COF a promising material for water treatment applications.
KW - COFs
KW - Ball-milling
KW - PFAS
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-648712
DO - https://doi.org/10.1002/smll.202509275
SN - 1613-6810
VL - 21
IS - 44
SP - 1
EP - 8
PB - Wiley
CY - Weinheim
AN - OPUS4-64871
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Dalgic, Mete‐Sungur
A1 - Kumar, Sourabh
A1 - Weidner, Steffen
T1 - Quantitative Analysis of Polymers by MALDI‐TOF Mass Spectrometry: Correlation Between Signal Intensity and Arm Number
N2 - The signal intensities of linear and star‐shaped poly(L‐lactides) (PLA) and poly (ethylene oxides) (PEO) were compared to determine the influence of the number of arms on the ionization in matrix‐assisted laser desorption/ionization time‐of‐flight (MALDI‐TOF) mass spectrometry. In this study, a variety of blends were prepared and investigated, including binary and ternary combinations of linear and star‐shaped polymers with similar molecular masses. The focus was on examining their intensity ratios. In equimolar binary PLA blends, polymer stars were observed to exhibit higher intensities than their linear counterparts. This result was supported by experiments with equimolar ternary PLA blends, which clearly demonstrated an intensity dependence on the number of polymer arms. It was observed that four‐arm PLA exhibited higher intensities than three‐arm PLA. A similar trend was observed in investigations involving acetylated polymer end groups, suggesting that differences in ionization are primarily influenced by polymer architecture rather than end groups. In order to validate this assumption, the binding energies for [polymer‐K] + adduct ions utilizing the most stable geometry obtained from GOAT (Global Optimizer Algorithm) were calculated, revealing that star‐shaped lower mass oligomers have slightly higher binding energies.
KW - MALDI-TOF MS
KW - Starlike polymers
KW - Quantification
KW - Topology
PY - 2026
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-653401
DO - https://doi.org/10.1002/jms.70023
SN - 1076-5174
VL - 61
IS - 1
SP - 1
EP - 12
PB - John Wiley & Sons Ltd.
AN - OPUS4-65340
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Weidner, Steffen
A1 - Meyer, Andreas
A1 - Falkenhagen, Jana
A1 - Kricheldorf, Hans R.
T1 - Cyclic polyglycolide by means of metal acetylacetonates
N2 - Glycolide was polymerized in bulk at 160 °C using various metal acetylacetonates as catalysts. Zirconium acetylacetonate was particularly efficient, enabling rapid polymerization even at 130 °C. The formation of cyclic poly(glycolic acid) (PGA), most likely via a ring-expansion polymerization (REP) mechanism, was proven by matrix-assisted laser desorption/ionization time-of-flight (MALDI-TOF) mass spectrometry. Depending on the polymerization conditions, the formation of even-numbered cycles was favored to varying degrees. Number-average molecular weights (Mn) in the range of 2000–3500 g mol−1 were achieved with dispersities below 2.0. Wide-angle X-ray scattering (WAXS) powder patterns showed that the crystal lattice was the same as that of known linear PGAs, regardless of the Mn values. These patterns enabled a comparison of crystallinities with values derived from DSC measurements.
KW - MALDI-TOF MS
KW - Polyglycolide
KW - Crystallization
KW - Small-angle X-ray scattering
KW - Cyclization
PY - 2026
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-653731
DO - https://doi.org/10.1039/d5ra07961f
SN - 2046-2069
VL - 16
IS - 2
SP - 1757
EP - 1764
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-65373
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - RPRT
A1 - Falkenhagen, Jana
A1 - Beskers, Timo. F.
A1 - Myxa, Anett
A1 - Pursch, Matthias
T1 - Round-robin test for size exclusion chromatography – Data summary
N2 - Size exclusion chromatography (SEC or GPC) is one critical component of polymer analysis to meet the increasing requirements in regulatory context – namely, determination of Mn, as well as oligomers of less than 500 g mol-1 and 1000 g mol-1. The underlying test methods (OECD 118/119 and DIN EN ISO 13885 1 to 3) provide a framework for SEC measurements; however, they lack sufficient specificity to obtain accurate results. Previous SEC round robin tests were mostly performed on homopolymers and did not collect data on oligomer contents.
A new round robin test was initiated and conceptualized within the Task force “Method Evaluation for Polymer REACh (MeEP)”, an initiative of “Industrieforum Analytik” within the German Chemical Society (GDCh). Samples for this study were selected to represent both easy benchmark polymers as well as real-life, industry-relevant polymer materials. Data collection focused on the regulatory requirements.
Distribution of samples, gathering of individual results and evaluation were carried out by BAM. A data summary as initial result is reported here. Further evaluation and interpretation are a part of ongoing research.
KW - Size exclusion chromatography
KW - Polymers
KW - Oligomer content
KW - Round-robin test
PY - 2026
DO - https://doi.org/10.26272/opus4-65587
SP - 1
EP - 84
PB - Bundesanstalt für Materialforschung und -prüfung (BAM)
CY - Berlin
AN - OPUS4-65587
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - CONF
A1 - Cakir, Cafer Tufan
T1 - Algorithm-Assisted Multimodal Synchrotron Experiments: XRD–XES Integration and SpecTwin
N2 - Multimodal synchrotron-based techniques are emerging as powerful tools for advanced materials characterization, enabling simultaneous insights into both crystal and electronic structure. We present a combined X-ray diffraction (XRD) and high-resolution X-ray emission spectroscopy (XES) approach implemented in a double-dispersive setup. This configuration enables simultaneous acquisition of structural and spectroscopic information with high precision, allowing us to resolve correlations between lattice arrangements and electronic configurations under in situ conditions.
To enhance experimental throughput and reproducibility, we employ digital twin concepts and optimization algorithms for experiment design and parameter control. These methods effectively eliminate trial-and-error procedures when optimizing the setup to achieve the desired resolution for XES analysis. In addition, we introduce SpecTwin, a dedicated software environment that integrates XES data analysis, simulation, and optimization routines.
This combined methodology underscores the potential of algorithm-assisted multimodal X-ray experiments to advance the quantitative understanding of structure–property relationships in complex materials.
T2 - Joint BAM-HZB Symposium on Multimodal Synchrotron Experiments for Next-Generation Materials Research
CY - Berlin, Germany
DA - 25.02.2026
KW - XAS
KW - Digital Twin
KW - Optimization
KW - Multimodal
PY - 2026
AN - OPUS4-65608
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -